# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_x8_11120 #TrackingRef 'X8_11120-silacycle.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H42 Cl2 N4 O7 S Si' _chemical_formula_weight 797.81 _chemical_absolute_configuration ad 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' Si Si 0.0817 0.0704 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.7839(4) _cell_length_b 16.5231(8) _cell_length_c 24.2524(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3920.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9380 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 30.40 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9282 _exptl_absorpt_correction_T_max 0.9704 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. Please acknowledge this grant in all publications of this structure. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 84425 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 29.80 _reflns_number_total 11230 _reflns_number_gt 10212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0497P)^2^+2.4005P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(6) _refine_ls_number_reflns 11230 _refine_ls_number_parameters 536 _refine_ls_number_restraints 146 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.105 _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 -0.14664(6) -0.16680(4) -0.21822(2) 0.02944(12) Uani 1 1 d . . . N1 N -0.14889(18) -0.13771(11) -0.15255(7) 0.0211(3) Uani 1 1 d . . . O1 O 0.19582(19) -0.23322(11) -0.16787(7) 0.0340(4) Uani 1 1 d . . . O2 O -0.09449(18) -0.29415(10) 0.01193(7) 0.0307(4) Uani 1 1 d . . . C2 C -0.0117(2) -0.12375(12) -0.12578(8) 0.0176(3) Uani 1 1 d . . . H2 H 0.0542 -0.0978 -0.1519 0.021 Uiso 1 1 calc R . . O3 O -0.07002(15) -0.09706(9) 0.02404(6) 0.0191(3) Uani 1 1 d . B . C3 C -0.04686(19) -0.06657(11) -0.07654(8) 0.0163(3) Uani 1 1 d . . . O4 O -0.0575(2) -0.23469(11) -0.22072(7) 0.0374(4) Uani 1 1 d . . . C4 C -0.1800(2) -0.02899(12) -0.09339(8) 0.0186(4) Uani 1 1 d . . . O5 O -0.2866(2) -0.17417(13) -0.23507(7) 0.0428(5) Uani 1 1 d . . . C5 C -0.2480(2) 0.03547(13) -0.06984(10) 0.0248(4) Uani 1 1 d . . . H5 H -0.2052 0.0676 -0.0423 0.030 Uiso 1 1 calc R . . C6 C -0.3806(2) 0.05247(15) -0.08727(11) 0.0322(5) Uani 1 1 d . . . H6 H -0.4289 0.0969 -0.0719 0.039 Uiso 1 1 calc R . . C7 C -0.4419(3) 0.00490(16) -0.12681(11) 0.0361(6) Uani 1 1 d . . . H7 H -0.5327 0.0171 -0.1379 0.043 Uiso 1 1 calc R . . C8 C -0.3749(2) -0.06057(15) -0.15102(10) 0.0300(5) Uani 1 1 d . . . H8 H -0.4189 -0.0940 -0.1775 0.036 Uiso 1 1 calc R . . C9 C -0.2405(2) -0.07469(13) -0.13471(8) 0.0224(4) Uani 1 1 d . . . N10 N 0.04591(19) -0.19483(10) -0.10055(7) 0.0198(3) Uani 1 1 d . . . C11 C 0.0328(2) -0.19491(12) -0.04014(8) 0.0178(4) Uani 1 1 d . . . H11 H 0.1219 -0.1785 -0.0233 0.021 Uiso 1 1 calc R . . C12 C -0.0727(2) -0.12984(11) -0.02936(8) 0.0169(3) Uani 1 1 d . . . H12 H -0.1651 -0.1541 -0.0354 0.020 Uiso 1 1 calc R . . C13 C -0.0037(2) -0.27994(12) -0.02116(9) 0.0222(4) Uani 1 1 d . . . N14 N 0.0747(2) -0.33599(11) -0.04640(8) 0.0266(4) Uani 1 1 d . . . C15 C 0.1821(2) -0.31273(13) -0.08510(9) 0.0272(4) Uani 1 1 d . . . H15A H 0.2060 -0.3603 -0.1080 0.033 Uiso 1 1 calc R . . H15B H 0.2646 -0.2973 -0.0640 0.033 Uiso 1 1 calc R . . C16 C 0.1431(2) -0.24297(13) -0.12299(9) 0.0242(4) Uani 1 1 d . . . C17 C 0.0587(3) -0.42206(13) -0.03312(12) 0.0371(6) Uani 1 1 d . . . H17A H -0.0044 -0.4280 -0.0020 0.056 Uiso 1 1 calc R . . H17B H 0.1477 -0.4450 -0.0232 0.056 Uiso 1 1 calc R . . H17C H 0.0220 -0.4507 -0.0652 0.056 Uiso 1 1 calc R . . C18 C -0.0727(3) -0.08533(16) -0.25405(9) 0.0320(5) Uani 1 1 d . . . C19 C 0.0651(3) -0.08724(17) -0.26785(10) 0.0363(5) Uani 1 1 d . . . H19 H 0.1191 -0.1336 -0.2599 0.044 Uiso 1 1 calc R . . C20 C 0.1223(3) -0.02049(19) -0.29329(11) 0.0433(7) Uani 1 1 d . . . H20 H 0.2157 -0.0216 -0.3040 0.052 Uiso 1 1 calc R . . C21 C 0.0445(4) 0.0480(2) -0.30338(11) 0.0478(7) Uani 1 1 d . . . H21 H 0.0855 0.0941 -0.3200 0.057 Uiso 1 1 calc R . . C22 C -0.0926(3) 0.0496(2) -0.28943(11) 0.0505(8) Uani 1 1 d . . . H22 H -0.1453 0.0967 -0.2966 0.061 Uiso 1 1 calc R . . C23 C -0.1532(3) -0.01684(19) -0.26513(11) 0.0438(7) Uani 1 1 d . . . H23 H -0.2477 -0.0163 -0.2561 0.053 Uiso 1 1 calc R . . N1' N 0.22544(17) 0.06213(10) -0.01741(8) 0.0207(3) Uani 1 1 d . . . C2' C 0.1253(2) 0.00134(11) -0.01246(8) 0.0182(4) Uani 1 1 d . B . C3' C 0.0663(2) -0.00849(11) -0.06320(8) 0.0163(3) Uani 1 1 d . . . C4' C 0.1264(2) 0.04902(12) -0.10126(8) 0.0193(4) Uani 1 1 d . . . C5' C 0.0978(2) 0.07013(13) -0.15575(9) 0.0252(4) Uani 1 1 d . . . H5' H 0.0298 0.0420 -0.1761 0.030 Uiso 1 1 calc R . . C6' C 0.1707(3) 0.13320(14) -0.17964(11) 0.0329(5) Uani 1 1 d . . . H6' H 0.1521 0.1485 -0.2166 0.039 Uiso 1 1 calc R . . O6' O 0.27926(18) 0.05652(11) 0.07365(7) 0.0337(4) Uani 1 1 d . . . C7' C 0.2706(2) 0.17416(14) -0.14992(11) 0.0316(5) Uani 1 1 d . . . H7' H 0.3196 0.2166 -0.1674 0.038 Uiso 1 1 calc R . . C8' C 0.3008(2) 0.15535(13) -0.09608(11) 0.0280(5) Uani 1 1 d . . . H8' H 0.3690 0.1840 -0.0761 0.034 Uiso 1 1 calc R . . C9' C 0.2268(2) 0.09207(12) -0.07189(9) 0.0213(4) Uani 1 1 d . . . C10' C 0.2955(2) 0.08849(13) 0.02922(10) 0.0270(4) Uani 1 1 d . A . O7' O 0.3735(2) 0.15039(11) 0.01714(8) 0.0397(4) Uani 1 1 d DU . . C11' C 0.4826(17) 0.1885(10) 0.0522(8) 0.0441(11) Uani 0.193(10) 1 d PDU A 1 C12' C 0.564(2) 0.2422(12) 0.0139(9) 0.0597(15) Uani 0.193(10) 1 d PDU A 1 H12A H 0.6368 0.2105 -0.0034 0.090 Uiso 0.193(10) 1 calc PR A 1 H12B H 0.6038 0.2869 0.0350 0.090 Uiso 0.193(10) 1 calc PR A 1 H12C H 0.5033 0.2640 -0.0147 0.090 Uiso 0.193(10) 1 calc PR A 1 C13' C 0.566(3) 0.1248(16) 0.0814(14) 0.0553(13) Uani 0.193(10) 1 d PDU A 1 H13A H 0.5952 0.0835 0.0549 0.083 Uiso 0.193(10) 1 calc PR A 1 H13B H 0.5106 0.0994 0.1103 0.083 Uiso 0.193(10) 1 calc PR A 1 H13C H 0.6468 0.1500 0.0981 0.083 Uiso 0.193(10) 1 calc PR A 1 C14' C 0.395(2) 0.2358(12) 0.0926(9) 0.0512(13) Uani 0.193(10) 1 d PDU A 1 H14A H 0.4492 0.2800 0.1085 0.077 Uiso 0.193(10) 1 calc PR A 1 H14B H 0.3640 0.1998 0.1222 0.077 Uiso 0.193(10) 1 calc PR A 1 H14C H 0.3158 0.2583 0.0733 0.077 Uiso 0.193(10) 1 calc PR A 1 C11B C 0.4426(5) 0.1969(2) 0.0627(2) 0.0441(11) Uani 0.807(10) 1 d PD A 2 C12B C 0.4999(6) 0.2668(3) 0.0307(2) 0.0597(15) Uani 0.807(10) 1 d PD A 2 H12D H 0.5699 0.2471 0.0051 0.090 Uiso 0.807(10) 1 calc PR A 2 H12E H 0.5408 0.3058 0.0563 0.090 Uiso 0.807(10) 1 calc PR A 2 H12F H 0.4264 0.2931 0.0099 0.090 Uiso 0.807(10) 1 calc PR A 2 C13B C 0.5554(7) 0.1422(3) 0.0866(3) 0.0553(13) Uani 0.807(10) 1 d PD A 2 H13D H 0.5134 0.0975 0.1070 0.083 Uiso 0.807(10) 1 calc PR A 2 H13E H 0.6134 0.1739 0.1115 0.083 Uiso 0.807(10) 1 calc PR A 2 H13F H 0.6111 0.1204 0.0565 0.083 Uiso 0.807(10) 1 calc PR A 2 C14B C 0.3435(6) 0.2251(3) 0.1063(2) 0.0512(13) Uani 0.807(10) 1 d PD A 2 H14D H 0.2744 0.2602 0.0894 0.077 Uiso 0.807(10) 1 calc PR A 2 H14E H 0.3930 0.2554 0.1347 0.077 Uiso 0.807(10) 1 calc PR A 2 H14F H 0.2988 0.1781 0.1230 0.077 Uiso 0.807(10) 1 calc PR A 2 C15' C 0.1815(3) -0.12217(16) 0.08508(10) 0.0323(5) Uani 1 1 d . B . H15C H 0.2343 -0.1504 0.0560 0.039 Uiso 1 1 calc R . . H15D H 0.2471 -0.0923 0.1086 0.039 Uiso 1 1 calc R . . C16' C 0.1070(4) -0.1851(2) 0.12030(15) 0.0579(9) Uani 1 1 d . . . H16A H 0.0508 -0.1576 0.1480 0.087 Uiso 1 1 calc R . . H16B H 0.1742 -0.2197 0.1388 0.087 Uiso 1 1 calc R . . H16C H 0.0485 -0.2184 0.0966 0.087 Uiso 1 1 calc R . . Si1 Si 0.06315(6) -0.04831(4) 0.05191(2) 0.02151(12) Uani 1 1 d DU . . C17' C -0.0150(4) 0.0131(2) 0.10756(14) 0.0300(7) Uani 0.755(5) 1 d PDU B 1 H17D H -0.0848 -0.0201 0.1266 0.036 Uiso 0.755(5) 1 calc PR B 1 H17E H 0.0566 0.0268 0.1349 0.036 Uiso 0.755(5) 1 calc PR B 1 C18' C -0.0803(6) 0.0897(3) 0.08819(19) 0.0633(13) Uani 0.755(5) 1 d PDU B 1 H18A H -0.0107 0.1249 0.0717 0.095 Uiso 0.755(5) 1 calc PR B 1 H18B H -0.1227 0.1174 0.1195 0.095 Uiso 0.755(5) 1 calc PR B 1 H18C H -0.1503 0.0770 0.0606 0.095 Uiso 0.755(5) 1 calc PR B 1 C17A C -0.0264(12) 0.0405(7) 0.0892(4) 0.0300(7) Uani 0.245(5) 1 d PDU B 2 H17F H 0.0417 0.0835 0.0965 0.036 Uiso 0.245(5) 1 calc PR B 2 H17G H -0.0972 0.0633 0.0646 0.036 Uiso 0.245(5) 1 calc PR B 2 C18A C -0.0915(16) 0.0168(10) 0.1423(5) 0.0633(13) Uani 0.245(5) 1 d PDU B 2 H18D H -0.1457 -0.0324 0.1369 0.095 Uiso 0.245(5) 1 calc PR B 2 H18E H -0.1512 0.0606 0.1551 0.095 Uiso 0.245(5) 1 calc PR B 2 H18F H -0.0205 0.0066 0.1700 0.095 Uiso 0.245(5) 1 calc PR B 2 C1S C -0.4328(7) 0.2453(3) -0.2496(2) 0.0252(12) Uani 0.488(5) 1 d PDU C 1 H1S1 H -0.5299 0.2371 -0.2596 0.030 Uiso 0.488(5) 1 calc PR C 1 H1S2 H -0.3791 0.2484 -0.2842 0.030 Uiso 0.488(5) 1 calc PR C 1 Cl1 Cl -0.41581(18) 0.33799(11) -0.21278(10) 0.0506(7) Uani 0.488(5) 1 d PDU C 1 Cl2 Cl -0.3764(2) 0.16377(16) -0.21068(10) 0.0622(7) Uani 0.488(5) 1 d PDU C 1 C2S C -0.434(2) 0.2325(8) -0.2531(6) 0.128(5) Uani 0.512(5) 1 d PDU C 2 H1S3 H -0.5251 0.2484 -0.2668 0.154 Uiso 0.512(5) 1 calc PR C 2 H1S4 H -0.3654 0.2478 -0.2813 0.154 Uiso 0.512(5) 1 calc PR C 2 Cl3 Cl -0.3980(5) 0.2860(7) -0.1903(2) 0.235(5) Uani 0.512(5) 1 d PDU C 2 Cl4 Cl -0.4296(9) 0.1266(5) -0.2433(3) 0.239(5) Uani 0.512(5) 1 d PDU 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 0.0365(3) 0.0332(3) 0.0186(2) -0.0035(2) -0.0072(2) -0.0033(2) N1 0.0230(8) 0.0233(8) 0.0171(7) -0.0001(6) -0.0055(7) -0.0006(7) O1 0.0401(10) 0.0368(9) 0.0251(8) -0.0053(7) 0.0051(7) 0.0111(8) O2 0.0355(9) 0.0218(7) 0.0348(9) 0.0078(6) 0.0035(7) -0.0028(6) C2 0.0212(9) 0.0170(8) 0.0147(8) -0.0008(6) -0.0020(7) 0.0001(7) O3 0.0198(6) 0.0218(6) 0.0156(6) -0.0016(5) 0.0002(5) -0.0031(5) C3 0.0166(8) 0.0148(8) 0.0176(8) 0.0000(6) -0.0006(7) 0.0004(6) O4 0.0527(11) 0.0318(9) 0.0277(8) -0.0122(7) -0.0064(8) 0.0015(8) C4 0.0176(8) 0.0169(8) 0.0213(9) 0.0057(7) -0.0009(7) 0.0003(7) O5 0.0411(10) 0.0599(13) 0.0273(9) -0.0022(9) -0.0134(8) -0.0118(10) C5 0.0228(10) 0.0212(10) 0.0303(10) 0.0033(8) 0.0003(8) 0.0020(8) C6 0.0259(10) 0.0309(11) 0.0397(12) 0.0088(10) 0.0020(9) 0.0100(9) C7 0.0234(11) 0.0409(14) 0.0441(14) 0.0126(11) -0.0065(10) 0.0079(10) C8 0.0228(10) 0.0347(12) 0.0327(11) 0.0063(9) -0.0094(9) -0.0007(9) C9 0.0247(10) 0.0236(10) 0.0189(9) 0.0050(7) -0.0040(7) 0.0009(8) N10 0.0259(9) 0.0173(7) 0.0164(7) -0.0010(6) -0.0010(6) 0.0045(7) C11 0.0185(9) 0.0180(8) 0.0169(8) 0.0004(7) -0.0022(7) 0.0015(7) C12 0.0192(8) 0.0152(8) 0.0162(8) 0.0001(6) -0.0008(7) -0.0006(7) C13 0.0270(10) 0.0163(9) 0.0235(10) 0.0037(7) -0.0070(8) 0.0008(8) N14 0.0335(10) 0.0159(8) 0.0303(9) 0.0006(7) -0.0063(8) 0.0039(7) C15 0.0319(11) 0.0231(10) 0.0267(10) -0.0042(8) -0.0030(9) 0.0096(9) C16 0.0273(10) 0.0219(9) 0.0233(9) -0.0060(7) -0.0016(8) 0.0063(8) C17 0.0472(15) 0.0144(9) 0.0497(14) 0.0019(9) -0.0120(12) 0.0035(10) C18 0.0400(13) 0.0398(13) 0.0162(9) 0.0024(9) -0.0017(9) 0.0007(11) C19 0.0437(14) 0.0427(14) 0.0225(10) -0.0018(9) 0.0063(10) 0.0052(12) C20 0.0468(16) 0.0545(17) 0.0285(12) 0.0022(11) 0.0120(11) 0.0008(13) C21 0.065(2) 0.0512(17) 0.0271(12) 0.0125(12) 0.0151(13) 0.0022(16) C22 0.0606(19) 0.0599(18) 0.0308(13) 0.0212(13) 0.0085(12) 0.0149(16) C23 0.0454(16) 0.0572(17) 0.0289(12) 0.0177(12) 0.0017(11) 0.0101(14) N1' 0.0177(7) 0.0165(8) 0.0277(9) -0.0007(7) -0.0017(7) -0.0018(6) C2' 0.0179(9) 0.0128(8) 0.0240(9) -0.0014(7) -0.0001(7) -0.0005(7) C3' 0.0162(8) 0.0138(8) 0.0190(8) -0.0002(6) 0.0024(7) 0.0005(7) C4' 0.0184(8) 0.0147(8) 0.0249(9) -0.0001(7) 0.0034(7) 0.0017(7) C5' 0.0299(11) 0.0200(9) 0.0256(10) 0.0040(8) 0.0052(8) 0.0021(8) C6' 0.0435(14) 0.0236(11) 0.0316(12) 0.0081(9) 0.0117(10) 0.0042(10) O6' 0.0357(9) 0.0302(8) 0.0353(9) -0.0042(7) -0.0120(7) -0.0040(7) C7' 0.0292(11) 0.0187(10) 0.0468(14) 0.0101(9) 0.0161(10) 0.0009(9) C8' 0.0193(9) 0.0179(9) 0.0469(13) 0.0000(9) 0.0075(9) 0.0005(8) C9' 0.0172(9) 0.0149(8) 0.0319(10) 0.0011(8) 0.0053(8) 0.0016(7) C10' 0.0230(10) 0.0181(9) 0.0399(12) -0.0033(9) -0.0087(9) 0.0019(8) O7' 0.0403(10) 0.0253(8) 0.0534(11) -0.0004(8) -0.0150(9) -0.0167(7) C11' 0.038(2) 0.0238(15) 0.070(3) -0.0087(15) -0.022(2) -0.0096(17) C12' 0.054(3) 0.038(2) 0.087(3) -0.001(2) -0.016(2) -0.027(2) C13' 0.042(2) 0.037(3) 0.087(3) -0.011(2) -0.031(2) -0.007(2) C14' 0.056(3) 0.0317(18) 0.066(3) -0.0155(18) -0.021(2) 0.000(2) C11B 0.038(2) 0.0238(15) 0.070(3) -0.0087(15) -0.022(2) -0.0096(17) C12B 0.054(3) 0.038(2) 0.087(3) -0.001(2) -0.016(2) -0.027(2) C13B 0.042(2) 0.037(3) 0.087(3) -0.011(2) -0.031(2) -0.007(2) C14B 0.056(3) 0.0317(18) 0.066(3) -0.0155(18) -0.021(2) 0.000(2) C15' 0.0329(12) 0.0404(13) 0.0236(11) 0.0077(9) -0.0092(9) -0.0055(10) C16' 0.063(2) 0.0505(18) 0.060(2) 0.0297(16) -0.0088(17) -0.0081(16) Si1 0.0217(3) 0.0258(3) 0.0170(2) -0.0044(2) 0.0006(2) -0.0032(2) C17' 0.0349(15) 0.0340(19) 0.0211(16) -0.0059(12) 0.0014(13) 0.0014(14) C18' 0.069(3) 0.070(3) 0.050(2) -0.016(2) -0.007(2) 0.045(2) C17A 0.0349(15) 0.0340(19) 0.0211(16) -0.0059(12) 0.0014(13) 0.0014(14) C18A 0.069(3) 0.070(3) 0.050(2) -0.016(2) -0.007(2) 0.045(2) C1S 0.018(2) 0.037(2) 0.021(2) -0.0084(19) 0.010(2) 0.002(2) Cl1 0.0366(8) 0.0569(11) 0.0583(12) -0.0298(8) -0.0140(7) 0.0052(7) Cl2 0.0601(12) 0.0664(13) 0.0601(13) 0.0225(10) 0.0102(9) 0.0153(10) C2S 0.123(12) 0.177(9) 0.085(9) 0.002(8) -0.014(9) 0.063(11) Cl3 0.106(3) 0.510(13) 0.088(3) -0.055(5) 0.005(2) -0.129(6) Cl4 0.292(8) 0.210(5) 0.214(6) 0.155(5) 0.180(6) 0.197(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 1.422(2) . ? S1 O5 1.4342(19) . ? S1 N1 1.6636(18) . ? S1 C18 1.758(3) . ? N1 C9 1.441(3) . ? N1 C2 1.509(3) . ? O1 C16 1.215(3) . ? O2 C13 1.220(3) . ? C2 N10 1.439(2) . ? C2 C3 1.561(3) . ? O3 C12 1.404(2) . ? O3 Si1 1.6743(15) . ? C3 C4 1.499(3) . ? C3 C3' 1.500(3) . ? C3 C12 1.570(3) . ? C4 C5 1.380(3) . ? C4 C9 1.388(3) . ? C5 C6 1.394(3) . ? C6 C7 1.377(4) . ? C7 C8 1.395(4) . ? C8 C9 1.392(3) . ? N10 C16 1.354(3) . ? N10 C11 1.471(2) . ? C11 C12 1.514(3) . ? C11 C13 1.521(3) . ? C13 N14 1.349(3) . ? N14 C15 1.460(3) . ? N14 C17 1.467(3) . ? C15 C16 1.523(3) . ? C18 C19 1.390(4) . ? C18 C23 1.405(4) . ? C19 C20 1.382(4) . ? C20 C21 1.385(4) . ? C21 C22 1.384(5) . ? C22 C23 1.380(4) . ? N1' C10' 1.392(3) . ? N1' C2' 1.408(2) . ? N1' C9' 1.411(3) . ? C2' C3' 1.369(3) . ? C2' Si1 1.866(2) . ? C3' C4' 1.450(3) . ? C4' C5' 1.395(3) . ? C4' C9' 1.406(3) . ? C5' C6' 1.389(3) . ? C6' C7' 1.390(4) . ? O6' C10' 1.211(3) . ? C7' C8' 1.374(4) . ? C8' C9' 1.401(3) . ? C10' O7' 1.310(3) . ? O7' C11' 1.503(14) . ? O7' C11B 1.506(4) . ? C11' C12' 1.510(13) . ? C11' C13' 1.510(14) . ? C11' C14' 1.518(13) . ? C11B C12B 1.498(6) . ? C11B C14B 1.509(6) . ? C11B C13B 1.540(6) . ? C15' C16' 1.530(4) . ? C15' Si1 1.864(3) . ? Si1 C17' 1.854(3) . ? Si1 C17A 1.934(10) . ? C17' C18' 1.493(6) . ? C17A C18A 1.489(14) . ? C1S Cl2 1.736(7) . ? C1S Cl1 1.781(5) . ? C2S Cl4 1.765(13) . ? C2S Cl3 1.796(13) . ? 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 O5 120.43(12) . . ? O4 S1 N1 106.07(10) . . ? O5 S1 N1 106.53(11) . . ? O4 S1 C18 109.29(13) . . ? O5 S1 C18 108.49(12) . . ? N1 S1 C18 104.92(10) . . ? C9 N1 C2 108.30(16) . . ? C9 N1 S1 120.31(14) . . ? C2 N1 S1 116.37(13) . . ? N10 C2 N1 113.99(16) . . ? N10 C2 C3 104.77(15) . . ? N1 C2 C3 103.03(15) . . ? C12 O3 Si1 124.93(13) . . ? C4 C3 C3' 115.76(15) . . ? C4 C3 C2 103.51(15) . . ? C3' C3 C2 112.92(15) . . ? C4 C3 C12 109.53(15) . . ? C3' C3 C12 112.80(15) . . ? C2 C3 C12 100.95(14) . . ? C5 C4 C9 120.87(19) . . ? C5 C4 C3 128.73(19) . . ? C9 C4 C3 110.03(17) . . ? C4 C5 C6 118.6(2) . . ? C7 C6 C5 120.1(2) . . ? C6 C7 C8 122.1(2) . . ? C9 C8 C7 117.0(2) . . ? C4 C9 C8 121.1(2) . . ? C4 C9 N1 110.15(18) . . ? C8 C9 N1 128.6(2) . . ? C16 N10 C2 125.69(18) . . ? C16 N10 C11 117.45(17) . . ? C2 N10 C11 112.98(15) . . ? N10 C11 C12 103.33(15) . . ? N10 C11 C13 108.84(16) . . ? C12 C11 C13 116.33(17) . . ? O3 C12 C11 114.86(16) . . ? O3 C12 C3 114.35(15) . . ? C11 C12 C3 103.72(15) . . ? O2 C13 N14 125.5(2) . . ? O2 C13 C11 123.23(19) . . ? N14 C13 C11 111.28(19) . . ? C13 N14 C15 121.34(18) . . ? C13 N14 C17 120.3(2) . . ? C15 N14 C17 118.3(2) . . ? N14 C15 C16 114.02(18) . . ? O1 C16 N10 125.5(2) . . ? O1 C16 C15 122.3(2) . . ? N10 C16 C15 112.21(19) . . ? C19 C18 C23 121.1(3) . . ? C19 C18 S1 120.1(2) . . ? C23 C18 S1 118.7(2) . . ? C20 C19 C18 118.8(3) . . ? C19 C20 C21 120.6(3) . . ? C22 C21 C20 120.3(3) . . ? C23 C22 C21 120.4(3) . . ? C22 C23 C18 118.8(3) . . ? C10' N1' C2' 119.75(18) . . ? C10' N1' C9' 130.27(18) . . ? C2' N1' C9' 109.67(17) . . ? C3' C2' N1' 107.55(17) . . ? C3' C2' Si1 124.22(15) . . ? N1' C2' Si1 127.73(15) . . ? C2' C3' C4' 108.86(17) . . ? C2' C3' C3 125.53(17) . . ? C4' C3' C3 125.55(17) . . ? C5' C4' C9' 119.58(19) . . ? C5' C4' C3' 133.27(19) . . ? C9' C4' C3' 107.00(17) . . ? C6' C5' C4' 118.6(2) . . ? C5' C6' C7' 120.7(2) . . ? C8' C7' C6' 122.3(2) . . ? C7' C8' C9' 117.1(2) . . ? C8' C9' C4' 121.8(2) . . ? C8' C9' N1' 131.2(2) . . ? C4' C9' N1' 106.88(17) . . ? O6' C10' O7' 128.0(2) . . ? O6' C10' N1' 121.5(2) . . ? O7' C10' N1' 110.5(2) . . ? C10' O7' C11' 127.9(7) . . ? C10' O7' C11B 119.8(3) . . ? C11' O7' C11B 18.6(7) . . ? O7' C11' C12' 105.8(12) . . ? O7' C11' C13' 111.0(16) . . ? C12' C11' C13' 114.4(16) . . ? O7' C11' C14' 100.4(12) . . ? C12' C11' C14' 113.0(14) . . ? C13' C11' C14' 111.2(16) . . ? C12B C11B O7' 100.5(3) . . ? C12B C11B C14B 111.4(4) . . ? O7' C11B C14B 112.5(3) . . ? C12B C11B C13B 112.3(4) . . ? O7' C11B C13B 107.3(3) . . ? C14B C11B C13B 112.2(4) . . ? C16' C15' Si1 113.0(2) . . ? O3 Si1 C17' 103.68(13) . . ? O3 Si1 C15' 110.03(10) . . ? C17' Si1 C15' 107.48(15) . . ? O3 Si1 C2' 97.33(8) . . ? C17' Si1 C2' 120.19(14) . . ? C15' Si1 C2' 116.51(10) . . ? O3 Si1 C17A 101.6(4) . . ? C17' Si1 C17A 19.4(3) . . ? C15' Si1 C17A 125.2(4) . . ? C2' Si1 C17A 101.9(3) . . ? C18' C17' Si1 114.3(3) . . ? C18A C17A Si1 113.6(8) . . ? Cl2 C1S Cl1 111.4(3) . . ? Cl4 C2S Cl3 111.7(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.80 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.359 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.058 _database_code_depnum_ccdc_archive 'CCDC 933935' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_x8_12215 #TrackingRef 'X8_12215-nitrobenzoylated12OHtrypt.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.33 H36.66 Cl0.66 N4 O10 S Si' _chemical_formula_weight 724.82 _chemical_absolute_configuration ad 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' Si Si 0.0817 0.0704 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 13.7346(10) _cell_length_b 16.0038(11) _cell_length_c 17.3585(13) _cell_angle_alpha 100.0100(10) _cell_angle_beta 92.2140(10) _cell_angle_gamma 108.5900(10) _cell_volume 3543.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9511 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 29.97 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1519 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9434 _exptl_absorpt_correction_T_max 0.9610 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. Please acknowledge this grant in all publications of this structure. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 106332 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.70 _reflns_number_total 36113 _reflns_number_gt 28476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1262P)^2^+2.3012P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(6) _refine_ls_number_reflns 36113 _refine_ls_number_parameters 2057 _refine_ls_number_restraints 2892 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2202 _refine_ls_wR_factor_gt 0.2013 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1A S 0.43581(8) 0.97344(6) 0.94798(7) 0.0489(2) Uani 1 1 d U . . N1A N 0.4962(3) 1.0019(2) 0.8696(2) 0.0443(7) Uani 1 1 d U . . C2A C 0.5998(3) 1.0065(2) 0.8601(3) 0.0463(8) Uani 1 1 d U . . H2A H 0.6402 0.9835 0.8908 0.056 Uiso 1 1 calc R . . C3A C 0.6318(3) 1.0495(2) 0.7995(2) 0.0394(7) Uani 1 1 d U . . C4A C 0.5472(3) 1.0744(2) 0.7696(2) 0.0376(7) Uani 1 1 d U . . C5A C 0.5338(3) 1.1151(2) 0.7073(2) 0.0380(7) Uani 1 1 d U . . H5A H 0.5883 1.1347 0.6756 0.046 Uiso 1 1 calc R . . C6A C 0.4392(3) 1.1263(3) 0.6923(2) 0.0444(8) Uani 1 1 d U . . H6A H 0.4287 1.1533 0.6495 0.053 Uiso 1 1 calc R . . C7A C 0.3591(3) 1.0984(3) 0.7395(2) 0.0475(9) Uani 1 1 d U . . H7A H 0.2953 1.1074 0.7283 0.057 Uiso 1 1 calc R . . C8A C 0.3705(3) 1.0582(3) 0.8015(2) 0.0452(8) Uani 1 1 d U . . H8A H 0.3163 1.0401 0.8337 0.054 Uiso 1 1 calc R . . C9A C 0.4649(3) 1.0453(2) 0.8152(2) 0.0393(7) Uani 1 1 d U . . N10A N 0.8730(2) 1.1756(2) 0.7173(2) 0.0404(6) Uani 1 1 d DU . . H10A H 0.935(2) 1.196(3) 0.744(3) 0.048 Uiso 1 1 d D . . C11A C 0.7953(3) 1.1648(2) 0.7720(2) 0.0403(7) Uani 1 1 d U . . H11A H 0.7465 1.1965 0.7593 0.048 Uiso 1 1 calc R . . C12A C 0.7346(3) 1.0640(3) 0.7670(3) 0.0453(8) Uani 1 1 d U B . H12A H 0.7227 1.0329 0.7106 0.054 Uiso 1 1 calc R . . O13A O 0.7955(2) 1.02702(19) 0.8089(2) 0.0526(7) Uani 1 1 d DU . . C14A C 0.8492(3) 1.2069(2) 0.8529(2) 0.0429(8) Uani 1 1 d U . . C15A C 0.8465(3) 1.1700(2) 0.6399(2) 0.0415(7) Uani 1 1 d U . . C16A C 0.9297(3) 1.1745(2) 0.5864(2) 0.0416(7) Uani 1 1 d U . . C17A C 1.0259(3) 1.1704(3) 0.6092(3) 0.0442(8) Uani 1 1 d U . . H17A H 1.0424 1.1656 0.6615 0.053 Uiso 1 1 calc R . . C18A C 1.0961(3) 1.1734(3) 0.5559(3) 0.0486(9) Uani 1 1 d U . . C19A C 1.0782(3) 1.1821(3) 0.4789(3) 0.0511(9) Uani 1 1 d U . . H19A H 1.1285 1.1842 0.4426 0.061 Uiso 1 1 calc R . . C20A C 0.9821(3) 1.1874(3) 0.4584(3) 0.0484(9) Uani 1 1 d U . . C21A C 0.9082(3) 1.1839(2) 0.5094(2) 0.0434(8) Uani 1 1 d U . . H21A H 0.8433 1.1877 0.4930 0.052 Uiso 1 1 calc R . . N22A N 0.9619(3) 1.2036(3) 0.3794(2) 0.0621(11) Uani 1 1 d U . . O23A O 0.8796(3) 1.2119(3) 0.3622(2) 0.0704(10) Uani 1 1 d U . . O24A O 1.0301(3) 1.2095(4) 0.3353(3) 0.0925(15) Uani 1 1 d U . . N25A N 1.1984(3) 1.1698(3) 0.5813(3) 0.0672(11) Uani 1 1 d U . . O26A O 1.2181(3) 1.1771(5) 0.6518(3) 0.1046(19) Uani 1 1 d U . . O27A O 1.2582(3) 1.1648(3) 0.5336(3) 0.0689(10) Uani 1 1 d U . . O28A O 0.7811(2) 1.2194(2) 0.90362(19) 0.0543(7) Uani 1 1 d DU A . C29A C 0.8186(4) 1.2504(4) 0.9860(3) 0.0691(13) Uani 1 1 d DU . . H29A H 0.8808 1.2343 0.9974 0.083 Uiso 0.604(13) 1 calc PR A 1 H29B H 0.7649 1.2225 1.0189 0.083 Uiso 0.604(13) 1 calc PR A 1 H29I H 0.8947 1.2775 0.9909 0.083 Uiso 0.396(13) 1 calc PR A 2 H29J H 0.8013 1.1981 1.0123 0.083 Uiso 0.396(13) 1 calc PR A 2 C30A C 0.8447(17) 1.3525(10) 1.0035(11) 0.094(3) Uani 0.396(13) 1 d PDU A 1 H30A H 0.8962 1.3791 0.9694 0.141 Uiso 0.396(13) 1 calc PR A 1 H30B H 0.8724 1.3764 1.0586 0.141 Uiso 0.396(13) 1 calc PR A 1 H30C H 0.7820 1.3674 0.9935 0.141 Uiso 0.396(13) 1 calc PR A 1 C30E C 0.7737(11) 1.3190(10) 1.0278(7) 0.094(3) Uani 0.604(13) 1 d PDU A 2 H30D H 0.8058 1.3770 1.0124 0.141 Uiso 0.604(13) 1 calc PR A 2 H30E H 0.7874 1.3259 1.0848 0.141 Uiso 0.604(13) 1 calc PR A 2 H30F H 0.6990 1.2985 1.0133 0.141 Uiso 0.604(13) 1 calc PR A 2 Si1A Si 0.82816(16) 0.93560(12) 0.78424(14) 0.0551(5) Uani 0.749(4) 1 d PDU B 1 C31A C 0.8406(7) 0.9186(5) 0.6762(4) 0.0728(18) Uani 0.749(4) 1 d PDU B 1 H31A H 0.7776 0.8730 0.6481 0.109 Uiso 0.749(4) 1 calc PR B 1 H31B H 0.8999 0.8985 0.6655 0.109 Uiso 0.749(4) 1 calc PR B 1 H31C H 0.8507 0.9754 0.6585 0.109 Uiso 0.749(4) 1 calc PR B 1 C32A C 0.7327(9) 0.8333(5) 0.8058(7) 0.097(2) Uani 0.749(4) 1 d PDU B 1 H32A H 0.7358 0.8364 0.8627 0.146 Uiso 0.749(4) 1 calc PR B 1 H32B H 0.7486 0.7801 0.7803 0.146 Uiso 0.749(4) 1 calc PR B 1 H32C H 0.6633 0.8291 0.7857 0.146 Uiso 0.749(4) 1 calc PR B 1 C33A C 0.9530(7) 0.9617(6) 0.8473(5) 0.0823(19) Uani 0.749(4) 1 d PDU B 1 C34A C 1.0419(7) 1.0296(7) 0.8140(8) 0.101(3) Uani 0.749(4) 1 d PDU B 1 H34A H 1.0241 1.0838 0.8115 0.152 Uiso 0.749(4) 1 calc PR B 1 H34B H 1.0513 1.0019 0.7612 0.152 Uiso 0.749(4) 1 calc PR B 1 H34C H 1.1060 1.0459 0.8485 0.152 Uiso 0.749(4) 1 calc PR B 1 C35A C 0.9792(10) 0.8749(8) 0.8500(6) 0.101(3) Uani 0.749(4) 1 d PDU B 1 H35A H 1.0471 0.8906 0.8792 0.152 Uiso 0.749(4) 1 calc PR B 1 H35B H 0.9801 0.8438 0.7963 0.152 Uiso 0.749(4) 1 calc PR B 1 H35C H 0.9268 0.8354 0.8763 0.152 Uiso 0.749(4) 1 calc PR B 1 C36A C 0.9452(10) 1.0045(8) 0.9324(5) 0.106(3) Uani 0.749(4) 1 d PDU B 1 H36A H 0.8888 0.9632 0.9540 0.159 Uiso 0.749(4) 1 calc PR B 1 H36B H 0.9315 1.0610 0.9329 0.159 Uiso 0.749(4) 1 calc PR B 1 H36C H 1.0103 1.0164 0.9643 0.159 Uiso 0.749(4) 1 calc PR B 1 Si1E Si 0.8494(5) 0.9494(4) 0.7585(4) 0.0551(5) Uani 0.251(4) 1 d PDU B 2 C31E C 0.9388(17) 0.9910(14) 0.6890(12) 0.0728(18) Uani 0.251(4) 1 d PDU B 2 H31D H 0.9029 0.9717 0.6358 0.109 Uiso 0.251(4) 1 calc PR B 2 H31E H 0.9959 0.9669 0.6913 0.109 Uiso 0.251(4) 1 calc PR B 2 H31F H 0.9661 1.0568 0.7022 0.109 Uiso 0.251(4) 1 calc PR B 2 C32E C 0.7422(16) 0.8481(10) 0.7076(14) 0.097(2) Uani 0.251(4) 1 d PDU B 2 H32D H 0.6941 0.8259 0.7455 0.146 Uiso 0.1255(19) 1 calc PR B 2 H32E H 0.7704 0.8012 0.6850 0.146 Uiso 0.1255(19) 1 calc PR B 2 H32F H 0.7057 0.8638 0.6657 0.146 Uiso 0.1255(19) 1 calc PR B 2 H32G H 0.7527 0.8347 0.6519 0.146 Uiso 0.1255(19) 1 calc PR B 2 H32H H 0.6764 0.8593 0.7124 0.146 Uiso 0.1255(19) 1 calc PR B 2 H32I H 0.7411 0.7968 0.7317 0.146 Uiso 0.1255(19) 1 calc PR B 2 C33E C 0.9080(16) 0.9253(14) 0.8469(10) 0.0823(19) Uani 0.251(4) 1 d PDU B 2 C34E C 1.0119(17) 1.0027(18) 0.872(2) 0.101(3) Uani 0.251(4) 1 d PDU B 2 H34D H 1.0559 1.0047 0.8292 0.152 Uiso 0.1255(19) 1 calc PR B 2 H34E H 1.0467 0.9924 0.9185 0.152 Uiso 0.1255(19) 1 calc PR B 2 H34F H 0.9989 1.0600 0.8857 0.152 Uiso 0.1255(19) 1 calc PR B 2 H34G H 1.0117 1.0334 0.9264 0.152 Uiso 0.1255(19) 1 calc PR B 2 H34H H 1.0210 1.0456 0.8371 0.152 Uiso 0.1255(19) 1 calc PR B 2 H34I H 1.0688 0.9781 0.8699 0.152 Uiso 0.1255(19) 1 calc PR B 2 C35E C 0.839(2) 0.923(2) 0.9154(14) 0.101(3) Uani 0.251(4) 1 d PDU B 2 H35D H 0.7666 0.9001 0.8943 0.152 Uiso 0.251(4) 1 calc PR B 2 H35E H 0.8557 0.9837 0.9467 0.152 Uiso 0.251(4) 1 calc PR B 2 H35F H 0.8524 0.8833 0.9487 0.152 Uiso 0.251(4) 1 calc PR B 2 C36E C 0.928(3) 0.8348(18) 0.8218(17) 0.106(3) Uani 0.251(4) 1 d PDU B 2 H36D H 0.9801 0.8416 0.7840 0.159 Uiso 0.251(4) 1 calc PR B 2 H36E H 0.8639 0.7880 0.7974 0.159 Uiso 0.251(4) 1 calc PR B 2 H36F H 0.9536 0.8177 0.8682 0.159 Uiso 0.251(4) 1 calc PR B 2 C37A C 0.4675(4) 1.0740(3) 1.0173(3) 0.0528(9) Uani 1 1 d U . . C38A C 0.4039(6) 1.1290(4) 1.0193(4) 0.0771(16) Uani 1 1 d U . . H38A H 0.3429 1.1101 0.9840 0.093 Uiso 1 1 calc R . . C39A C 0.4299(7) 1.2088(4) 1.0717(4) 0.0857(19) Uani 1 1 d U . . H39A H 0.3885 1.2464 1.0724 0.103 Uiso 1 1 calc R . . C40A C 0.5195(6) 1.2343(4) 1.1248(3) 0.0790(16) Uani 1 1 d U . . H40A H 0.5376 1.2890 1.1623 0.095 Uiso 1 1 calc R . . C41A C 0.5777(6) 1.1839(4) 1.1232(4) 0.0835(18) Uani 1 1 d U . . H41A H 0.6369 1.2023 1.1603 0.100 Uiso 1 1 calc R . . C42A C 0.5554(5) 1.1026(3) 1.0678(3) 0.0660(12) Uani 1 1 d U . . H42A H 0.6008 1.0684 1.0659 0.079 Uiso 1 1 calc R . . O43A O 0.4837(3) 0.9174(2) 0.9768(2) 0.0621(8) Uani 1 1 d U . . O44A O 0.3278(3) 0.9426(2) 0.9224(2) 0.0577(8) Uani 1 1 d U . . O45A O 0.9401(2) 1.2264(2) 0.86996(18) 0.0483(6) Uani 1 1 d U . . O46A O 0.7577(2) 1.1573(2) 0.61461(18) 0.0512(7) Uani 1 1 d U . . Si1B Si 0.54338(9) 0.59686(8) 0.49698(7) 0.0495(3) Uani 1 1 d U . . S1B S 0.14130(10) 0.52881(8) 0.29058(8) 0.0611(3) Uani 1 1 d U . . N1B N 0.1743(3) 0.5089(3) 0.3763(2) 0.0566(9) Uani 1 1 d U . . C2B C 0.2725(3) 0.5060(3) 0.3943(2) 0.0509(9) Uani 1 1 d U . . H2B H 0.3301 0.5262 0.3656 0.061 Uiso 1 1 calc R . . C3B C 0.2732(3) 0.4698(2) 0.4589(2) 0.0429(8) Uani 1 1 d U . . C4B C 0.1696(3) 0.4479(2) 0.4830(2) 0.0430(8) Uani 1 1 d U . . C5B C 0.1257(3) 0.4108(2) 0.5471(2) 0.0405(7) Uani 1 1 d U . . H5B H 0.1654 0.3928 0.5829 0.049 Uiso 1 1 calc R . . C6B C 0.0228(3) 0.4013(3) 0.5560(3) 0.0489(9) Uani 1 1 d U . . H6B H -0.0077 0.3772 0.5990 0.059 Uiso 1 1 calc R . . C7B C -0.0358(3) 0.4261(3) 0.5041(3) 0.0573(11) Uani 1 1 d U . . H7B H -0.1058 0.4189 0.5121 0.069 Uiso 1 1 calc R . . C8B C 0.0053(4) 0.4614(3) 0.4401(3) 0.0611(11) Uani 1 1 d U . . H8B H -0.0354 0.4777 0.4037 0.073 Uiso 1 1 calc R . . C9B C 0.1087(3) 0.4718(3) 0.4316(3) 0.0504(9) Uani 1 1 d U . . N10B N 0.4303(3) 0.3544(3) 0.5559(2) 0.0495(8) Uani 1 1 d DU . . H10B H 0.474(3) 0.328(3) 0.536(3) 0.059 Uiso 1 1 d D . . C11B C 0.3536(3) 0.3599(3) 0.4992(3) 0.0498(9) Uani 1 1 d U . . H11B H 0.2833 0.3281 0.5133 0.060 Uiso 1 1 calc R . . C12B C 0.3639(3) 0.4593(3) 0.4999(2) 0.0434(8) Uani 1 1 d U . . H12B H 0.3728 0.4916 0.5558 0.052 Uiso 1 1 calc R . . O13B O 0.4550(2) 0.4972(2) 0.46434(17) 0.0500(7) Uani 1 1 d U . . C14B C 0.3683(4) 0.3119(4) 0.4196(3) 0.0621(12) Uani 1 1 d U . . C15B C 0.4163(3) 0.3634(3) 0.6318(3) 0.0474(9) Uani 1 1 d U . . C16B C 0.4994(3) 0.3564(3) 0.6854(3) 0.0478(9) Uani 1 1 d U . . C17B C 0.6001(3) 0.3691(3) 0.6647(3) 0.0472(8) Uani 1 1 d U . . H17B H 0.6181 0.3827 0.6149 0.057 Uiso 1 1 calc R . . C18B C 0.6720(3) 0.3617(3) 0.7176(3) 0.0510(9) Uani 1 1 d U . . C19B C 0.6492(4) 0.3393(3) 0.7904(3) 0.0544(10) Uani 1 1 d U . . H19B H 0.6996 0.3328 0.8258 0.065 Uiso 1 1 calc R . . C20B C 0.5483(4) 0.3270(3) 0.8084(3) 0.0556(10) Uani 1 1 d U . . C21B C 0.4739(4) 0.3369(3) 0.7586(3) 0.0506(9) Uani 1 1 d U . . H21B H 0.4066 0.3306 0.7739 0.061 Uiso 1 1 calc R . . N22B N 0.5173(4) 0.2982(3) 0.8828(3) 0.0635(10) Uani 1 1 d U . . O23B O 0.4313(3) 0.2919(3) 0.8996(2) 0.0681(9) Uani 1 1 d U . . O24B O 0.5816(5) 0.2827(4) 0.9236(3) 0.1027(18) Uani 1 1 d U . . N25B N 0.7784(3) 0.3762(3) 0.6955(3) 0.0623(10) Uani 1 1 d U . . O26B O 0.7953(3) 0.3965(4) 0.6299(3) 0.0834(12) Uani 1 1 d U . . O27B O 0.8426(3) 0.3686(2) 0.7419(3) 0.0735(10) Uani 1 1 d U . . O28B O 0.2876(3) 0.2983(3) 0.3692(2) 0.0731(10) Uani 1 1 d DU C . C29B C 0.2958(6) 0.2579(5) 0.2885(4) 0.090(2) Uani 1 1 d DU . . H29C H 0.3237 0.2080 0.2884 0.108 Uiso 0.757(12) 1 calc PR C 1 H29D H 0.2267 0.2334 0.2584 0.108 Uiso 0.757(12) 1 calc PR C 1 H29K H 0.3176 0.3066 0.2582 0.108 Uiso 0.243(12) 1 calc PR C 2 H29L H 0.3514 0.2311 0.2896 0.108 Uiso 0.243(12) 1 calc PR C 2 C30B C 0.3581(10) 0.3207(7) 0.2557(4) 0.098(3) Uani 0.757(12) 1 d PDU C 1 H30G H 0.3483 0.3007 0.1984 0.147 Uiso 0.757(12) 1 calc PR C 1 H30H H 0.4299 0.3312 0.2747 0.147 Uiso 0.757(12) 1 calc PR C 1 H30I H 0.3421 0.3766 0.2696 0.147 Uiso 0.757(12) 1 calc PR C 1 C30F C 0.212(2) 0.1958(16) 0.2501(11) 0.098(3) Uani 0.243(12) 1 d PDU C 2 H30J H 0.2270 0.1732 0.1973 0.147 Uiso 0.121(6) 1 calc PR C 2 H30K H 0.1568 0.2218 0.2460 0.147 Uiso 0.121(6) 1 calc PR C 2 H30L H 0.1899 0.1461 0.2785 0.147 Uiso 0.121(6) 1 calc PR C 2 H30M H 0.1555 0.1876 0.2839 0.147 Uiso 0.121(6) 1 calc PR C 2 H30N H 0.2256 0.1389 0.2352 0.147 Uiso 0.121(6) 1 calc PR C 2 H30O H 0.1926 0.2146 0.2027 0.147 Uiso 0.121(6) 1 calc PR C 2 C31B C 0.5043(5) 0.6879(4) 0.4643(5) 0.0821(17) Uani 1 1 d U . . H31G H 0.4997 0.6789 0.4068 0.123 Uiso 1 1 calc R . . H31H H 0.5558 0.7465 0.4869 0.123 Uiso 1 1 calc R . . H31I H 0.4369 0.6862 0.4821 0.123 Uiso 1 1 calc R . . C32B C 0.5623(4) 0.6184(4) 0.6064(3) 0.0635(13) Uani 1 1 d U . . H32J H 0.5000 0.6260 0.6279 0.095 Uiso 1 1 calc R . . H32K H 0.6213 0.6732 0.6255 0.095 Uiso 1 1 calc R . . H32L H 0.5755 0.5674 0.6234 0.095 Uiso 1 1 calc R . . C33B C 0.6589(3) 0.5843(3) 0.4493(3) 0.0527(10) Uani 1 1 d U . . C34B C 0.7465(4) 0.6756(4) 0.4627(4) 0.0658(12) Uani 1 1 d U . . H34J H 0.7610 0.7013 0.5191 0.099 Uiso 1 1 calc R . . H34K H 0.7255 0.7167 0.4353 0.099 Uiso 1 1 calc R . . H34L H 0.8088 0.6670 0.4422 0.099 Uiso 1 1 calc R . . C35B C 0.6968(4) 0.5165(3) 0.4831(3) 0.0618(11) Uani 1 1 d U . . H35G H 0.7501 0.5031 0.4521 0.093 Uiso 1 1 calc R . . H35H H 0.6388 0.4611 0.4810 0.093 Uiso 1 1 calc R . . H35I H 0.7259 0.5421 0.5378 0.093 Uiso 1 1 calc R . . C36B C 0.6296(5) 0.5500(4) 0.3605(3) 0.0788(17) Uani 1 1 d U . . H36G H 0.6881 0.5380 0.3361 0.118 Uiso 1 1 calc R . . H36H H 0.6118 0.5956 0.3374 0.118 Uiso 1 1 calc R . . H36I H 0.5701 0.4945 0.3513 0.118 Uiso 1 1 calc R . . C37B C 0.0976(4) 0.4227(3) 0.2276(3) 0.0540(10) Uani 1 1 d U . . C38B C -0.0041(4) 0.3722(3) 0.2284(3) 0.0635(12) Uani 1 1 d U . . H38B H -0.0487 0.3931 0.2612 0.076 Uiso 1 1 calc R . . C39B C -0.0388(5) 0.2856(4) 0.1763(4) 0.0736(14) Uani 1 1 d U . . H39B H -0.1093 0.2490 0.1718 0.088 Uiso 1 1 calc R . . C40B C 0.0296(5) 0.2556(4) 0.1332(3) 0.0706(14) Uani 1 1 d U . . H40B H 0.0063 0.1972 0.1009 0.085 Uiso 1 1 calc R . . C41B C 0.1321(5) 0.3092(4) 0.1360(3) 0.0667(12) Uani 1 1 d U . . H41B H 0.1785 0.2881 0.1055 0.080 Uiso 1 1 calc R . . C42B C 0.1658(4) 0.3934(4) 0.1837(3) 0.0595(11) Uani 1 1 d U . . H42B H 0.2356 0.4309 0.1863 0.071 Uiso 1 1 calc R . . O43B O 0.2306(4) 0.5825(2) 0.2644(2) 0.0761(11) Uani 1 1 d U . . O44B O 0.0699(3) 0.56126(19) 0.30643(18) 0.0596(7) Uani 1 1 d U . . O45B O 0.4432(3) 0.2909(3) 0.4065(2) 0.0788(12) Uani 1 1 d U . . O46B O 0.3388(3) 0.3778(2) 0.6566(2) 0.0590(8) Uani 1 1 d U . . N1C N 0.4585(3) 0.4847(2) -0.0004(2) 0.0455(7) Uani 1 1 d U . . C2C C 0.3631(3) 0.4928(3) -0.0224(2) 0.0429(8) Uani 1 1 d U E . H2C H 0.3043 0.4782 0.0061 0.051 Uiso 1 1 calc R . . C3C C 0.3668(3) 0.5238(3) -0.0891(2) 0.0405(7) Uani 1 1 d U . . C4C C 0.4704(3) 0.5395(3) -0.1121(2) 0.0376(7) Uani 1 1 d U E . C5C C 0.5194(3) 0.5706(3) -0.1757(2) 0.0417(8) Uani 1 1 d U . . H5C H 0.4826 0.5866 -0.2150 0.050 Uiso 1 1 calc R E . C7C C 0.6763(3) 0.5537(3) -0.1224(3) 0.0473(9) Uani 1 1 d U . . H7C H 0.7467 0.5593 -0.1270 0.057 Uiso 1 1 calc R E . C6C C 0.6218(3) 0.5778(3) -0.1809(2) 0.0438(8) Uani 1 1 d U E . H6C H 0.6557 0.5990 -0.2239 0.053 Uiso 1 1 calc R . . C8C C 0.6306(3) 0.5225(3) -0.0593(2) 0.0453(8) Uani 1 1 d U E . H8C H 0.6680 0.5067 -0.0202 0.054 Uiso 1 1 calc R . . C9C C 0.5272(3) 0.5151(3) -0.0550(2) 0.0407(7) Uani 1 1 d U E . N10C N 0.1752(2) 0.5104(2) -0.25822(17) 0.0364(6) Uani 1 1 d DU E . H10C H 0.1099(18) 0.476(3) -0.265(3) 0.044 Uiso 1 1 d D . . C11C C 0.2425(3) 0.4774(2) -0.21467(19) 0.0352(7) Uani 1 1 d U . . H11C H 0.3042 0.4788 -0.2438 0.042 Uiso 1 1 calc R E . C12C C 0.2787(3) 0.5395(3) -0.1333(2) 0.0373(7) Uani 1 1 d U D . H12C H 0.3023 0.6032 -0.1408 0.045 Uiso 1 1 calc R . . O13C O 0.1929(2) 0.5268(2) -0.08884(15) 0.0425(6) Uani 1 1 d DU . . C14C C 0.1824(3) 0.3800(3) -0.21105(19) 0.0393(7) Uani 1 1 d U E . C15C C 0.2113(3) 0.5707(2) -0.30407(19) 0.0333(6) Uani 1 1 d U . . C16C C 0.1302(3) 0.6014(2) -0.3417(2) 0.0326(6) Uani 1 1 d U E . C17C C 0.0354(2) 0.5949(2) -0.3106(2) 0.0350(6) Uani 1 1 d U . . H17C H 0.0179 0.5673 -0.2665 0.042 Uiso 1 1 calc R E . C18C C -0.0312(3) 0.6292(2) -0.3451(2) 0.0389(7) Uani 1 1 d U E . C19C C -0.0114(3) 0.6664(3) -0.4111(3) 0.0491(9) Uani 1 1 d U . . H19C H -0.0590 0.6886 -0.4350 0.059 Uiso 1 1 calc R E . C20C C 0.0821(3) 0.6699(3) -0.4408(2) 0.0436(8) Uani 1 1 d U E . C21C C 0.1540(3) 0.6400(2) -0.4067(2) 0.0381(7) Uani 1 1 d U . . H21C H 0.2183 0.6459 -0.4275 0.046 Uiso 1 1 calc R E . N22C N 0.1034(4) 0.7058(4) -0.5121(3) 0.0686(12) Uani 1 1 d U . . O23C O 0.1909(3) 0.7180(3) -0.5333(2) 0.0819(13) Uani 1 1 d U E . O24C O 0.0355(4) 0.7222(4) -0.5470(3) 0.0964(16) Uani 1 1 d U E . N25C N -0.1282(3) 0.6256(3) -0.3102(2) 0.0513(8) Uani 1 1 d U . . O26C O -0.1498(3) 0.5823(3) -0.2580(3) 0.0745(11) Uani 1 1 d U E . O27C O -0.1787(3) 0.6657(3) -0.3340(2) 0.0738(11) Uani 1 1 d U E . O28C O 0.2402(2) 0.34552(18) -0.17254(15) 0.0427(6) Uani 1 1 d U . . C29C C 0.1918(4) 0.2557(3) -0.1564(2) 0.0466(8) Uani 1 1 d U E . H29E H 0.2336 0.2171 -0.1739 0.056 Uiso 1 1 calc R . . H29F H 0.1221 0.2281 -0.1852 0.056 Uiso 1 1 calc R . . C30C C 0.1842(4) 0.2638(4) -0.0689(2) 0.0580(11) Uani 1 1 d U . . H30P H 0.2537 0.2884 -0.0409 0.087 Uiso 1 1 calc R E . H30Q H 0.1490 0.2043 -0.0574 0.087 Uiso 1 1 calc R . . H30R H 0.1450 0.3040 -0.0517 0.087 Uiso 1 1 calc R . . C31C C 0.1331(10) 0.6808(7) -0.1063(6) 0.079(2) Uani 0.574(5) 1 d PDU D 1 H31J H 0.1530 0.6622 -0.1585 0.118 Uiso 0.574(5) 1 calc PR D 1 H31K H 0.1765 0.7427 -0.0840 0.118 Uiso 0.574(5) 1 calc PR D 1 H31L H 0.0605 0.6774 -0.1110 0.118 Uiso 0.574(5) 1 calc PR D 1 C32C C 0.2479(7) 0.6731(7) 0.0431(5) 0.0679(16) Uani 0.574(5) 1 d PDU D 1 H32M H 0.2795 0.6360 0.0676 0.102 Uiso 0.574(5) 1 calc PR D 1 H32N H 0.2143 0.7032 0.0823 0.102 Uiso 0.574(5) 1 calc PR D 1 H32O H 0.3014 0.7183 0.0226 0.102 Uiso 0.574(5) 1 calc PR D 1 Si1C Si 0.1515(4) 0.6014(4) -0.0379(3) 0.0565(9) Uani 0.574(5) 1 d PDU D 1 C33C C 0.0252(7) 0.5429(6) -0.0096(5) 0.0732(17) Uani 0.574(5) 1 d PDU D 1 C34C C -0.0306(8) 0.6124(8) 0.0180(7) 0.084(2) Uani 0.574(5) 1 d PDU D 1 H34M H 0.0050 0.6515 0.0677 0.127 Uiso 0.574(5) 1 calc PR D 1 H34N H -0.1023 0.5804 0.0256 0.127 Uiso 0.574(5) 1 calc PR D 1 H34O H -0.0297 0.6489 -0.0220 0.127 Uiso 0.574(5) 1 calc PR D 1 C35C C 0.0405(10) 0.4880(8) 0.0497(6) 0.098(3) Uani 0.574(5) 1 d PDU D 1 H35J H 0.0862 0.5280 0.0953 0.147 Uiso 0.574(5) 1 calc PR D 1 H35K H 0.0715 0.4438 0.0255 0.147 Uiso 0.574(5) 1 calc PR D 1 H35L H -0.0265 0.4568 0.0666 0.147 Uiso 0.574(5) 1 calc PR D 1 C36C C -0.0451(7) 0.4781(8) -0.0860(6) 0.087(2) Uani 0.574(5) 1 d PDU D 1 H36J H -0.0210 0.4269 -0.1020 0.131 Uiso 0.574(5) 1 calc PR D 1 H36K H -0.0405 0.5114 -0.1288 0.131 Uiso 0.574(5) 1 calc PR D 1 H36L H -0.1170 0.4563 -0.0741 0.131 Uiso 0.574(5) 1 calc PR D 1 C31G C 0.2909(10) 0.6997(8) 0.0134(8) 0.079(2) Uani 0.426(5) 1 d PDU D 2 H31M H 0.3410 0.6808 0.0416 0.118 Uiso 0.426(5) 1 calc PR D 2 H31N H 0.2759 0.7483 0.0481 0.118 Uiso 0.426(5) 1 calc PR D 2 H31O H 0.3197 0.7210 -0.0331 0.118 Uiso 0.426(5) 1 calc PR D 2 C32G C 0.1327(10) 0.5426(8) 0.0653(6) 0.0679(16) Uani 0.426(5) 1 d PDU D 2 H32P H 0.0962 0.5738 0.1011 0.102 Uiso 0.426(5) 1 calc PR D 2 H32Q H 0.1941 0.5402 0.0943 0.102 Uiso 0.426(5) 1 calc PR D 2 H32R H 0.0869 0.4813 0.0434 0.102 Uiso 0.426(5) 1 calc PR D 2 Si1G Si 0.1727(5) 0.6050(6) -0.0168(4) 0.0565(9) Uani 0.426(5) 1 d PDU D 2 C33G C 0.0647(8) 0.6362(7) -0.0572(6) 0.0732(17) Uani 0.426(5) 1 d PDU D 2 C34G C 0.1059(11) 0.6990(10) -0.1160(8) 0.084(2) Uani 0.426(5) 1 d PDU D 2 H34P H 0.0478 0.7082 -0.1438 0.127 Uiso 0.426(5) 1 calc PR D 2 H34Q H 0.1431 0.6714 -0.1540 0.127 Uiso 0.426(5) 1 calc PR D 2 H34R H 0.1528 0.7571 -0.0872 0.127 Uiso 0.426(5) 1 calc PR D 2 C35G C 0.0260(13) 0.6900(11) 0.0117(8) 0.098(3) Uani 0.426(5) 1 d PDU D 2 H35M H 0.0787 0.7121 0.0568 0.147 Uiso 0.426(5) 1 calc PR D 2 H35N H -0.0380 0.6506 0.0267 0.147 Uiso 0.426(5) 1 calc PR D 2 H35O H 0.0129 0.7410 -0.0054 0.147 Uiso 0.426(5) 1 calc PR D 2 C36G C -0.0226(8) 0.5505(9) -0.0971(9) 0.087(2) Uani 0.426(5) 1 d PDU D 2 H36M H -0.0809 0.5666 -0.1163 0.131 Uiso 0.426(5) 1 calc PR D 2 H36N H -0.0450 0.5113 -0.0591 0.131 Uiso 0.426(5) 1 calc PR D 2 H36O H 0.0024 0.5189 -0.1414 0.131 Uiso 0.426(5) 1 calc PR D 2 S1C S 0.48944(10) 0.46976(8) 0.08836(7) 0.0411(3) Uani 0.925(3) 1 d PDU E 1 O43C O 0.3940(3) 0.4147(2) 0.1110(2) 0.0509(7) Uani 0.925(3) 1 d PDU E 1 O44C O 0.5749(4) 0.4392(4) 0.0838(5) 0.0532(8) Uani 0.925(3) 1 d PDU E 1 C37C C 0.5227(3) 0.5765(3) 0.1482(2) 0.0444(9) Uani 0.925(3) 1 d PDU E 1 C38C C 0.6251(4) 0.6302(4) 0.1611(3) 0.0543(11) Uani 0.925(3) 1 d PDU E 1 H38C H 0.6773 0.6104 0.1377 0.065 Uiso 0.925(3) 1 calc PR E 1 C39C C 0.6498(5) 0.7164(3) 0.2109(3) 0.0661(13) Uani 0.925(3) 1 d PDU E 1 H39C H 0.7195 0.7553 0.2212 0.079 Uiso 0.925(3) 1 calc PR E 1 C40C C 0.5747(6) 0.7426(4) 0.2429(4) 0.0827(17) Uani 0.925(3) 1 d PDU E 1 H40C H 0.5923 0.8007 0.2752 0.099 Uiso 0.925(3) 1 calc PR E 1 C41C C 0.4725(6) 0.6882(4) 0.2308(5) 0.0860(19) Uani 0.925(3) 1 d PDU E 1 H41C H 0.4211 0.7084 0.2551 0.103 Uiso 0.925(3) 1 calc PR E 1 C42C C 0.4454(5) 0.6030(3) 0.1821(3) 0.0626(12) Uani 0.925(3) 1 d PDU E 1 H42C H 0.3756 0.5644 0.1726 0.075 Uiso 0.925(3) 1 calc PR E 1 S1G S 0.5286(13) 0.4977(10) 0.1100(9) 0.0411(3) Uani 0.075(3) 1 d PDU E 2 O43G O 0.4323(19) 0.466(2) 0.143(2) 0.0509(7) Uani 0.075(3) 1 d PDU E 2 O44G O 0.584(4) 0.438(4) 0.086(7) 0.0532(8) Uani 0.075(3) 1 d PDU E 2 C37G C 0.601(2) 0.589(2) 0.1824(19) 0.0444(9) Uani 0.075(3) 1 d PDU E 2 C38G C 0.698(2) 0.648(2) 0.182(2) 0.0543(11) Uani 0.075(3) 1 d PDU E 2 H38G H 0.7426 0.6344 0.1451 0.065 Uiso 0.075(3) 1 calc PR E 2 C39G C 0.733(3) 0.731(2) 0.239(2) 0.0661(13) Uani 0.075(3) 1 d PDU E 2 H39G H 0.8010 0.7723 0.2397 0.079 Uiso 0.075(3) 1 calc PR E 2 C40G C 0.668(4) 0.750(3) 0.290(3) 0.0827(17) Uani 0.075(3) 1 d PDU E 2 H40G H 0.6917 0.8055 0.3273 0.099 Uiso 0.075(3) 1 calc PR E 2 C41G C 0.571(4) 0.694(3) 0.291(3) 0.0860(19) Uani 0.075(3) 1 d PDU E 2 H41G H 0.5241 0.7113 0.3233 0.103 Uiso 0.075(3) 1 calc PR E 2 C42G C 0.541(3) 0.607(3) 0.242(2) 0.0626(12) Uani 0.075(3) 1 d PDU E 2 H42G H 0.4800 0.5618 0.2497 0.075 Uiso 0.075(3) 1 calc PR E 2 O45C O 0.0957(2) 0.3413(2) -0.24118(18) 0.0490(6) Uani 1 1 d U . . O46C O 0.30133(19) 0.60241(19) -0.31459(17) 0.0427(6) Uani 1 1 d U E . S1D S 0.81336(8) 1.02910(7) 0.17350(7) 0.0496(2) Uani 1 1 d U . . N1D N 0.7800(3) 1.0173(2) 0.2623(2) 0.0475(7) Uani 1 1 d U . . C2D C 0.6832(3) 1.0178(3) 0.2861(3) 0.0477(9) Uani 1 1 d U . . H2D H 0.6347 1.0355 0.2580 0.057 Uiso 1 1 calc R . . C3D C 0.6698(3) 0.9890(3) 0.3554(2) 0.0476(9) Uani 1 1 d U . . C4D C 0.7593(3) 0.9687(3) 0.3776(2) 0.0450(8) Uani 1 1 d U . . C5D C 0.7881(4) 0.9366(3) 0.4429(3) 0.0535(10) Uani 1 1 d U . . H5D H 0.7437 0.9252 0.4832 0.064 Uiso 1 1 calc R . . C6D C 0.8821(4) 0.9222(4) 0.4470(3) 0.0641(12) Uani 1 1 d U . . H6D H 0.9026 0.9009 0.4906 0.077 Uiso 1 1 calc R . . C7D C 0.9476(4) 0.9390(4) 0.3868(3) 0.0670(13) Uani 1 1 d U . . H7D H 1.0115 0.9281 0.3907 0.080 Uiso 1 1 calc R . . C8D C 0.9223(4) 0.9707(4) 0.3222(3) 0.0583(11) Uani 1 1 d U . . H8D H 0.9671 0.9822 0.2821 0.070 Uiso 1 1 calc R . . C9D C 0.8272(3) 0.9847(3) 0.3195(3) 0.0459(8) Uani 1 1 d U . . C11D C 0.5965(3) 1.0380(3) 0.4816(3) 0.0532(10) Uani 1 1 d U . . H11D H 0.6680 1.0444 0.5022 0.064 Uiso 1 1 calc R F 1 C12D C 0.5752(3) 0.9781(3) 0.3987(3) 0.0539(11) Uani 1 1 d U G . H12D H 0.5480 0.9140 0.4050 0.065 Uiso 1 1 calc R . . O13D O 0.4974(2) 0.9955(2) 0.35647(19) 0.0616(9) Uani 1 1 d DU . . C14D C 0.5951(3) 1.1317(3) 0.4802(2) 0.0508(9) Uani 1 1 d U G . N10D N 0.5228(7) 0.9909(7) 0.5380(6) 0.0405(15) Uani 0.575(8) 1 d PDU G 1 H10D H 0.4679 1.0070 0.5461 0.049 Uiso 0.575(8) 1 calc PR G 1 C15D C 0.5350(7) 0.9262(8) 0.5768(7) 0.0421(18) Uani 0.575(8) 1 d PDU G 1 O46D O 0.6093(7) 0.9016(8) 0.5736(6) 0.0501(15) Uani 0.575(8) 1 d PDU G 1 C16D C 0.4501(7) 0.8891(7) 0.6278(7) 0.053(2) Uani 0.575(8) 1 d PDU G 1 C17D C 0.4738(8) 0.8475(6) 0.6858(6) 0.055(2) Uani 0.575(8) 1 d PDU G 1 H17D H 0.5396 0.8402 0.6911 0.066 Uiso 0.575(8) 1 calc PR G 1 C18D C 0.4002(7) 0.8161(6) 0.7365(6) 0.0568(19) Uani 0.575(8) 1 d PDU G 1 C19D C 0.3054(7) 0.8242(6) 0.7324(6) 0.062(2) Uani 0.575(8) 1 d PDU G 1 H19D H 0.2571 0.8037 0.7684 0.074 Uiso 0.575(8) 1 calc PR G 1 C20D C 0.2826(7) 0.8642(7) 0.6728(6) 0.057(2) Uani 0.575(8) 1 d PDU G 1 C21D C 0.3535(6) 0.8968(6) 0.6201(5) 0.0496(18) Uani 0.575(8) 1 d PDU G 1 H21D H 0.3350 0.9237 0.5797 0.060 Uiso 0.575(8) 1 calc PR G 1 N22D N 0.1793(6) 0.8731(6) 0.6634(5) 0.066(2) Uani 0.575(8) 1 d PDU G 1 O23D O 0.1197(6) 0.8487(7) 0.7109(6) 0.086(3) Uani 0.575(8) 1 d PDU G 1 O24D O 0.1573(8) 0.9014(8) 0.6057(5) 0.078(3) Uani 0.575(8) 1 d PDU G 1 N25D N 0.4229(10) 0.7705(8) 0.7972(9) 0.073(3) Uani 0.575(8) 1 d PDU G 1 O26D O 0.3637(8) 0.7524(5) 0.8461(5) 0.081(2) Uani 0.575(8) 1 d PDU G 1 O27D O 0.5072(8) 0.7570(7) 0.7986(7) 0.093(3) Uani 0.575(8) 1 d PDU G 1 N10H N 0.5081(10) 1.0058(10) 0.5194(8) 0.0405(15) Uani 0.425(8) 1 d PDU G 2 H10H H 0.4538 1.0234 0.5165 0.049 Uiso 0.425(8) 1 calc PR G 2 C15H C 0.5167(10) 0.9432(11) 0.5618(10) 0.0421(18) Uani 0.425(8) 1 d PDU G 2 O46H O 0.5861(10) 0.9114(11) 0.5575(9) 0.0501(15) Uani 0.425(8) 1 d PDU G 2 C16H C 0.4280(9) 0.9089(9) 0.6086(8) 0.056(3) Uani 0.425(8) 1 d PDU G 2 C17H C 0.4413(11) 0.8576(9) 0.6618(9) 0.064(3) Uani 0.425(8) 1 d PDU G 2 H17H H 0.5031 0.8434 0.6667 0.077 Uiso 0.425(8) 1 calc PR G 2 C18H C 0.3611(12) 0.8269(8) 0.7084(8) 0.069(3) Uani 0.425(8) 1 d PDU G 2 C19H C 0.2707(12) 0.8436(10) 0.7005(10) 0.074(3) Uani 0.425(8) 1 d PDU G 2 H19H H 0.2168 0.8221 0.7321 0.089 Uiso 0.425(8) 1 calc PR G 2 C20H C 0.2602(10) 0.8917(9) 0.6463(9) 0.072(3) Uani 0.425(8) 1 d PDU G 2 C21H C 0.3377(10) 0.9257(9) 0.5987(9) 0.061(3) Uani 0.425(8) 1 d PDU G 2 H21H H 0.3275 0.9594 0.5610 0.073 Uiso 0.425(8) 1 calc PR G 2 N22H N 0.1640(12) 0.9151(12) 0.6387(10) 0.086(4) Uani 0.425(8) 1 d PDU G 2 O23H O 0.0913(12) 0.8738(9) 0.6708(12) 0.124(6) Uani 0.425(8) 1 d PDU G 2 O24H O 0.1588(9) 0.9631(12) 0.5930(10) 0.127(6) Uani 0.425(8) 1 d PDU G 2 N25H N 0.3776(12) 0.7801(10) 0.7704(9) 0.090(4) Uani 0.425(8) 1 d PDU G 2 O26H O 0.3062(13) 0.7493(6) 0.8081(7) 0.095(4) Uani 0.425(8) 1 d PDU G 2 O27H O 0.4614(12) 0.7695(13) 0.7788(11) 0.109(5) Uani 0.425(8) 1 d PDU G 2 O28D O 0.6664(2) 1.1721(2) 0.43764(18) 0.0514(7) Uani 1 1 d U . . C29D C 0.6715(4) 1.2617(3) 0.4250(3) 0.0592(11) Uani 1 1 d U G . H29G H 0.6184 1.2810 0.4528 0.071 Uiso 1 1 calc R . . H29H H 0.7402 1.3058 0.4459 0.071 Uiso 1 1 calc R . . C30D C 0.6538(6) 1.2572(5) 0.3409(4) 0.0846(18) Uani 1 1 d U . . H30S H 0.7122 1.2470 0.3148 0.127 Uiso 1 1 calc R G . H30T H 0.6470 1.3140 0.3319 0.127 Uiso 1 1 calc R . . H30U H 0.5902 1.2077 0.3193 0.127 Uiso 1 1 calc R . . C31D C 0.3327(12) 0.8399(10) 0.3588(11) 0.0813(19) Uani 0.421(6) 1 d PDU G 1 H31P H 0.3673 0.7967 0.3392 0.122 Uiso 0.421(6) 1 calc PR G 1 H31Q H 0.2582 0.8127 0.3437 0.122 Uiso 0.421(6) 1 calc PR G 1 H31R H 0.3457 0.8566 0.4163 0.122 Uiso 0.421(6) 1 calc PR G 1 C32D C 0.4261(17) 0.890(2) 0.2076(9) 0.091(3) Uani 0.421(6) 1 d PDU G 1 H32S H 0.3687 0.8751 0.1667 0.136 Uiso 0.421(6) 1 calc PR G 1 H32T H 0.4435 0.8354 0.2106 0.136 Uiso 0.421(6) 1 calc PR G 1 H32U H 0.4863 0.9357 0.1947 0.136 Uiso 0.421(6) 1 calc PR G 1 Si1D Si 0.3822(5) 0.9388(5) 0.3172(6) 0.106(2) Uani 0.421(6) 1 d PDU G 1 C33D C 0.2939(8) 0.9938(10) 0.2903(8) 0.097(2) Uani 0.421(6) 1 d PDU G 1 C34D C 0.3485(16) 1.0533(12) 0.2323(10) 0.114(3) Uani 0.421(6) 1 d PDU G 1 H34S H 0.2971 1.0681 0.2015 0.171 Uiso 0.421(6) 1 calc PR G 1 H34T H 0.3835 1.0204 0.1967 0.171 Uiso 0.421(6) 1 calc PR G 1 H34U H 0.3993 1.1088 0.2620 0.171 Uiso 0.421(6) 1 calc PR G 1 C35D C 0.2004(11) 0.9174(16) 0.2396(12) 0.138(5) Uani 0.421(6) 1 d PDU G 1 H35P H 0.1619 0.8779 0.2733 0.207 Uiso 0.211(3) 1 calc PR G 1 H35Q H 0.2260 0.8824 0.1981 0.207 Uiso 0.211(3) 1 calc PR G 1 H35R H 0.1548 0.9442 0.2157 0.207 Uiso 0.211(3) 1 calc PR G 1 H35S H 0.1999 0.9251 0.1848 0.207 Uiso 0.211(3) 1 calc PR G 1 H35T H 0.1358 0.9206 0.2599 0.207 Uiso 0.211(3) 1 calc PR G 1 H35U H 0.2070 0.8588 0.2424 0.207 Uiso 0.211(3) 1 calc PR G 1 C36D C 0.2763(14) 1.0376(14) 0.3751(11) 0.119(4) Uani 0.421(6) 1 d PDU G 1 H36P H 0.3139 1.1024 0.3855 0.178 Uiso 0.421(6) 1 calc PR G 1 H36Q H 0.3016 1.0102 0.4144 0.178 Uiso 0.421(6) 1 calc PR G 1 H36R H 0.2024 1.0273 0.3782 0.178 Uiso 0.421(6) 1 calc PR G 1 C31H C 0.3624(9) 0.8146(8) 0.3607(8) 0.0813(19) Uani 0.579(6) 1 d PDU G 2 H31S H 0.4146 0.7852 0.3510 0.122 Uiso 0.579(6) 1 calc PR G 2 H31T H 0.2940 0.7717 0.3400 0.122 Uiso 0.579(6) 1 calc PR G 2 H31U H 0.3637 0.8353 0.4174 0.122 Uiso 0.579(6) 1 calc PR G 2 C32H C 0.4003(12) 0.8951(14) 0.1970(6) 0.091(3) Uani 0.579(6) 1 d PDU G 2 H32V H 0.3867 0.9447 0.1777 0.136 Uiso 0.579(6) 1 calc PR G 2 H32W H 0.3494 0.8379 0.1702 0.136 Uiso 0.579(6) 1 calc PR G 2 H32X H 0.4698 0.8951 0.1861 0.136 Uiso 0.579(6) 1 calc PR G 2 Si1H Si 0.3902(3) 0.9101(3) 0.3120(3) 0.0762(12) Uani 0.579(6) 1 d PDU G 2 C33H C 0.2801(6) 0.9492(8) 0.3422(6) 0.097(2) Uani 0.579(6) 1 d PDU G 2 C34H C 0.2983(13) 1.0432(10) 0.3234(9) 0.114(3) Uani 0.579(6) 1 d PDU G 2 H34V H 0.2318 1.0526 0.3156 0.171 Uiso 0.579(6) 1 calc PR G 2 H34W H 0.3333 1.0479 0.2754 0.171 Uiso 0.579(6) 1 calc PR G 2 H34X H 0.3413 1.0890 0.3672 0.171 Uiso 0.579(6) 1 calc PR G 2 C35H C 0.1805(9) 0.8803(13) 0.2928(9) 0.138(5) Uani 0.579(6) 1 d PDU G 2 H35V H 0.1195 0.8907 0.3140 0.207 Uiso 0.579(6) 1 calc PR G 2 H35W H 0.1783 0.8190 0.2953 0.207 Uiso 0.579(6) 1 calc PR G 2 H35X H 0.1814 0.8878 0.2379 0.207 Uiso 0.579(6) 1 calc PR G 2 C36H C 0.2648(10) 0.9574(12) 0.4303(7) 0.119(4) Uani 0.579(6) 1 d PDU G 2 H36S H 0.2810 1.0209 0.4546 0.178 Uiso 0.579(6) 1 calc PR G 2 H36T H 0.3108 0.9323 0.4559 0.178 Uiso 0.579(6) 1 calc PR G 2 H36U H 0.1930 0.9243 0.4364 0.178 Uiso 0.579(6) 1 calc PR G 2 C37D C 0.7612(3) 0.9213(3) 0.1125(2) 0.0451(8) Uani 1 1 d U . . C38D C 0.6600(4) 0.8918(3) 0.0811(2) 0.0486(9) Uani 1 1 d U . . H38D H 0.6173 0.9276 0.0942 0.058 Uiso 1 1 calc R . . C39D C 0.6207(5) 0.8094(3) 0.0300(3) 0.0591(11) Uani 1 1 d U . . H39D H 0.5514 0.7890 0.0069 0.071 Uiso 1 1 calc R . . C40D C 0.6822(5) 0.7571(3) 0.0128(3) 0.0648(12) Uani 1 1 d U . . H40D H 0.6546 0.7000 -0.0214 0.078 Uiso 1 1 calc R . . C41D C 0.7812(5) 0.7859(4) 0.0438(4) 0.0723(14) Uani 1 1 d U . . H41D H 0.8226 0.7489 0.0308 0.087 Uiso 1 1 calc R . . C42D C 0.8248(5) 0.8697(4) 0.0952(4) 0.0668(13) Uani 1 1 d U . . H42D H 0.8948 0.8900 0.1171 0.080 Uiso 1 1 calc R . . O43D O 0.9237(3) 1.0563(3) 0.1793(2) 0.0699(10) Uani 1 1 d U . . O44D O 0.7605(3) 1.0848(2) 0.1490(2) 0.0609(8) Uani 1 1 d U . . O45D O 0.5369(2) 1.1637(3) 0.51468(18) 0.0602(9) Uani 1 1 d U . . Cl1S Cl -0.16303(15) 0.54481(14) 0.20302(14) 0.0738(7) Uani 0.693(5) 1 d PU . . Cl2S Cl -0.0675(2) 0.73700(16) 0.20793(13) 0.0884(9) Uani 0.693(5) 1 d PU . . C1S C -0.1015(8) 0.6491(6) 0.2584(5) 0.078(2) Uani 0.693(5) 1 d PU . . H1S1 H -0.0381 0.6479 0.2865 0.094 Uiso 0.693(5) 1 calc PR . . H1S2 H -0.1468 0.6620 0.2986 0.094 Uiso 0.693(5) 1 calc PR . . Cl3S Cl -0.9115(3) -0.1357(3) 0.0612(3) 0.1268(17) Uani 0.629(6) 1 d PU H 1 Cl4S Cl -0.8676(4) 0.0525(3) 0.1030(3) 0.142(2) Uani 0.629(6) 1 d PU H 1 C2S C -0.8234(12) -0.0331(10) 0.0567(10) 0.114(4) Uani 0.629(6) 1 d PU H 1 H2S1 H -0.8146 -0.0283 0.0011 0.137 Uiso 0.629(6) 1 calc PR H 1 H2S2 H -0.7557 -0.0269 0.0832 0.137 Uiso 0.629(6) 1 calc PR H 1 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 S1A 0.0537(5) 0.0331(4) 0.0598(6) 0.0087(4) 0.0082(4) 0.0140(4) N1A 0.0438(16) 0.0387(15) 0.0514(18) 0.0022(13) 0.0054(13) 0.0184(13) C2A 0.0417(18) 0.0302(16) 0.067(2) 0.0054(16) 0.0013(17) 0.0152(14) C3A 0.0366(16) 0.0278(15) 0.052(2) -0.0032(13) -0.0004(14) 0.0139(13) C4A 0.0368(16) 0.0273(14) 0.0439(17) -0.0083(12) -0.0016(13) 0.0127(13) C5A 0.0378(16) 0.0354(16) 0.0354(16) -0.0098(13) -0.0003(13) 0.0142(14) C6A 0.0464(19) 0.050(2) 0.0363(17) -0.0085(15) -0.0074(14) 0.0249(17) C7A 0.0433(19) 0.054(2) 0.048(2) -0.0041(16) -0.0019(15) 0.0270(17) C8A 0.0426(18) 0.0458(19) 0.0454(19) -0.0056(15) 0.0050(15) 0.0199(16) C9A 0.0395(17) 0.0355(16) 0.0414(17) -0.0063(13) 0.0007(13) 0.0181(14) N10A 0.0315(14) 0.0375(15) 0.0506(17) 0.0047(13) -0.0049(12) 0.0125(12) C11A 0.0314(15) 0.0323(15) 0.057(2) 0.0056(14) -0.0028(14) 0.0126(13) C12A 0.0360(17) 0.0341(16) 0.068(2) 0.0068(16) -0.0001(16) 0.0176(14) O13A 0.0435(14) 0.0398(14) 0.083(2) 0.0142(14) 0.0027(14) 0.0242(12) C14A 0.0428(18) 0.0336(16) 0.051(2) 0.0089(14) -0.0008(15) 0.0112(14) C15A 0.0353(16) 0.0325(16) 0.0513(19) -0.0001(14) -0.0083(14) 0.0096(13) C16A 0.0322(16) 0.0333(16) 0.0519(19) 0.0028(14) -0.0062(14) 0.0048(13) C17A 0.0373(17) 0.0424(18) 0.053(2) 0.0136(16) -0.0036(15) 0.0120(15) C18A 0.0358(17) 0.046(2) 0.064(2) 0.0177(18) 0.0017(16) 0.0100(16) C19A 0.0391(19) 0.049(2) 0.058(2) 0.0168(18) -0.0003(16) 0.0020(16) C20A 0.0408(19) 0.0404(19) 0.049(2) 0.0098(16) -0.0096(15) -0.0057(15) C21A 0.0320(16) 0.0350(17) 0.052(2) 0.0090(15) -0.0121(14) -0.0031(14) N22A 0.0438(19) 0.071(3) 0.052(2) 0.0170(18) -0.0098(16) -0.0092(17) O23A 0.0543(19) 0.083(2) 0.0568(19) 0.0165(17) -0.0168(15) -0.0003(17) O24A 0.058(2) 0.141(4) 0.067(2) 0.049(3) 0.0006(18) 0.002(2) N25A 0.049(2) 0.089(3) 0.084(3) 0.048(3) 0.0158(19) 0.033(2) O26A 0.056(2) 0.196(6) 0.100(3) 0.089(4) 0.018(2) 0.062(3) O27A 0.0498(18) 0.080(2) 0.094(3) 0.043(2) 0.0267(18) 0.0285(17) O28A 0.0474(15) 0.0617(18) 0.0523(16) 0.0014(14) 0.0042(12) 0.0211(14) C29A 0.063(3) 0.085(4) 0.054(2) 0.005(2) 0.011(2) 0.021(3) C30A 0.099(8) 0.104(6) 0.073(6) -0.024(5) -0.014(5) 0.049(6) C30E 0.099(8) 0.104(6) 0.073(6) -0.024(5) -0.014(5) 0.049(6) Si1A 0.0605(10) 0.0420(8) 0.0849(14) 0.0348(8) 0.0431(9) 0.0316(8) C31A 0.093(5) 0.069(4) 0.085(4) 0.027(3) 0.040(4) 0.055(4) C32A 0.122(6) 0.041(3) 0.131(6) 0.023(3) 0.059(5) 0.023(3) C33A 0.099(5) 0.086(5) 0.105(4) 0.050(4) 0.038(4) 0.071(4) C34A 0.068(4) 0.115(6) 0.142(8) 0.040(6) 0.011(4) 0.053(4) C35A 0.149(7) 0.125(7) 0.093(6) 0.060(5) 0.040(5) 0.109(6) C36A 0.158(9) 0.133(6) 0.073(4) 0.024(4) -0.004(4) 0.112(7) Si1E 0.0605(10) 0.0420(8) 0.0849(14) 0.0348(8) 0.0431(9) 0.0316(8) C31E 0.093(5) 0.069(4) 0.085(4) 0.027(3) 0.040(4) 0.055(4) C32E 0.122(6) 0.041(3) 0.131(6) 0.023(3) 0.059(5) 0.023(3) C33E 0.099(5) 0.086(5) 0.105(4) 0.050(4) 0.038(4) 0.071(4) C34E 0.068(4) 0.115(6) 0.142(8) 0.040(6) 0.011(4) 0.053(4) C35E 0.149(7) 0.125(7) 0.093(6) 0.060(5) 0.040(5) 0.109(6) C36E 0.158(9) 0.133(6) 0.073(4) 0.024(4) -0.004(4) 0.112(7) C37A 0.069(3) 0.0403(19) 0.048(2) 0.0079(16) 0.0086(18) 0.0170(18) C38A 0.123(5) 0.055(3) 0.065(3) 0.005(2) 0.002(3) 0.049(3) C39A 0.146(6) 0.061(3) 0.068(3) 0.006(2) 0.007(3) 0.063(4) C40A 0.122(5) 0.053(3) 0.061(3) -0.001(2) 0.010(3) 0.035(3) C41A 0.121(5) 0.048(3) 0.067(3) -0.003(2) -0.018(3) 0.019(3) C42A 0.088(3) 0.049(2) 0.064(3) 0.008(2) 0.015(2) 0.027(2) O43A 0.071(2) 0.0444(16) 0.078(2) 0.0202(15) 0.0112(17) 0.0240(15) O44A 0.0516(16) 0.0399(15) 0.076(2) 0.0089(14) 0.0104(15) 0.0089(13) O45A 0.0387(13) 0.0521(16) 0.0517(15) 0.0094(13) -0.0023(11) 0.0131(12) O46A 0.0344(13) 0.0536(16) 0.0578(17) -0.0029(13) -0.0104(12) 0.0128(12) Si1B 0.0437(5) 0.0422(5) 0.0527(6) -0.0034(5) 0.0021(5) 0.0073(4) S1B 0.0619(7) 0.0479(6) 0.0647(7) 0.0043(5) -0.0178(5) 0.0124(5) N1B 0.064(2) 0.0442(18) 0.0463(18) 0.0033(14) -0.0118(16) 0.0018(16) C2B 0.049(2) 0.049(2) 0.0407(19) -0.0027(16) 0.0000(16) 0.0031(17) C3B 0.0423(18) 0.0349(17) 0.0415(18) -0.0034(14) 0.0064(14) 0.0046(14) C4B 0.0414(18) 0.0350(17) 0.0423(18) -0.0051(14) 0.0016(14) 0.0055(14) C5B 0.0394(17) 0.0315(16) 0.0443(18) -0.0051(13) 0.0074(14) 0.0093(14) C6B 0.0378(18) 0.0344(17) 0.060(2) -0.0109(16) 0.0077(16) 0.0027(14) C7B 0.0347(18) 0.047(2) 0.075(3) -0.008(2) -0.0070(18) 0.0048(16) C8B 0.045(2) 0.052(2) 0.073(3) -0.005(2) -0.019(2) 0.0098(19) C9B 0.0439(19) 0.044(2) 0.049(2) -0.0013(16) -0.0119(16) 0.0025(16) N10B 0.0420(17) 0.0534(19) 0.0549(18) 0.0005(15) 0.0191(14) 0.0218(15) C11B 0.0396(18) 0.048(2) 0.058(2) -0.0045(17) 0.0146(16) 0.0146(16) C12B 0.0397(17) 0.0416(18) 0.0423(18) 0.0003(14) 0.0125(14) 0.0078(14) O13B 0.0406(14) 0.0494(15) 0.0460(15) -0.0038(12) 0.0122(11) 0.0016(12) C14B 0.058(3) 0.062(3) 0.061(3) -0.014(2) -0.001(2) 0.028(2) C15B 0.0426(19) 0.046(2) 0.054(2) 0.0007(17) 0.0217(16) 0.0178(16) C16B 0.048(2) 0.0411(19) 0.054(2) -0.0043(16) 0.0162(16) 0.0204(16) C17B 0.051(2) 0.0364(17) 0.055(2) 0.0003(16) 0.0173(17) 0.0183(16) C18B 0.047(2) 0.0383(18) 0.067(2) -0.0055(17) 0.0063(17) 0.0209(17) C19B 0.065(2) 0.041(2) 0.060(2) -0.0083(17) 0.0030(19) 0.0311(19) C20B 0.070(3) 0.046(2) 0.054(2) -0.0084(17) 0.0166(19) 0.032(2) C21B 0.059(2) 0.0426(19) 0.053(2) -0.0022(16) 0.0225(18) 0.0249(18) N22B 0.089(3) 0.055(2) 0.058(2) -0.0024(17) 0.015(2) 0.045(2) O23B 0.090(3) 0.069(2) 0.0539(18) 0.0048(16) 0.0235(18) 0.041(2) O24B 0.132(4) 0.146(5) 0.079(3) 0.027(3) 0.028(3) 0.111(4) N25B 0.049(2) 0.051(2) 0.088(3) 0.001(2) 0.0167(19) 0.0235(17) O26B 0.055(2) 0.113(4) 0.090(3) 0.016(3) 0.0237(19) 0.038(2) O27B 0.0513(18) 0.0547(19) 0.116(3) 0.0065(19) -0.0043(19) 0.0263(16) O28B 0.066(2) 0.067(2) 0.074(2) -0.0227(17) -0.0135(17) 0.0276(18) C29B 0.132(6) 0.078(4) 0.060(3) -0.009(3) -0.023(3) 0.050(4) C30B 0.167(8) 0.100(6) 0.038(3) 0.003(3) -0.012(4) 0.067(5) C30F 0.167(8) 0.100(6) 0.038(3) 0.003(3) -0.012(4) 0.067(5) C31B 0.071(3) 0.055(3) 0.108(5) -0.001(3) -0.024(3) 0.015(3) C32B 0.047(2) 0.080(3) 0.048(2) -0.011(2) 0.0062(18) 0.014(2) C33B 0.044(2) 0.049(2) 0.056(2) 0.0111(18) 0.0150(17) 0.0011(16) C34B 0.057(3) 0.058(3) 0.074(3) 0.024(2) 0.006(2) 0.003(2) C35B 0.052(2) 0.056(2) 0.077(3) 0.007(2) 0.023(2) 0.019(2) C36B 0.078(4) 0.083(4) 0.048(2) -0.001(2) 0.024(2) -0.004(3) C37B 0.060(2) 0.046(2) 0.047(2) 0.0065(16) -0.0138(18) 0.0083(18) C38B 0.055(2) 0.051(2) 0.075(3) 0.009(2) 0.004(2) 0.007(2) C39B 0.067(3) 0.060(3) 0.069(3) -0.001(2) -0.012(2) -0.004(2) C40B 0.088(4) 0.053(3) 0.055(3) 0.007(2) 0.001(2) 0.005(2) C41B 0.077(3) 0.064(3) 0.049(2) 0.006(2) 0.007(2) 0.012(2) C42B 0.064(3) 0.060(3) 0.048(2) 0.0149(19) 0.0017(19) 0.009(2) O43B 0.100(3) 0.0423(16) 0.067(2) 0.0177(15) -0.0113(19) -0.0035(17) O44B 0.100(2) 0.0289(12) 0.0485(15) -0.0010(11) 0.0072(16) 0.0232(14) O45B 0.073(2) 0.100(3) 0.065(2) -0.023(2) 0.0050(17) 0.051(2) O46B 0.0563(17) 0.071(2) 0.0639(19) 0.0112(16) 0.0287(15) 0.0391(16) N1C 0.0462(17) 0.0558(19) 0.0395(15) 0.0029(13) 0.0021(13) 0.0275(15) C2C 0.0387(17) 0.055(2) 0.0386(17) 0.0051(15) 0.0047(14) 0.0224(16) C3C 0.0346(16) 0.054(2) 0.0356(16) 0.0032(15) 0.0078(13) 0.0214(15) C4C 0.0352(16) 0.0441(18) 0.0349(16) -0.0037(13) 0.0052(13) 0.0210(14) C5C 0.0403(18) 0.0466(19) 0.0397(18) 0.0003(15) 0.0080(14) 0.0204(16) C7C 0.0333(17) 0.0429(19) 0.062(2) -0.0072(17) 0.0052(15) 0.0162(15) C6C 0.0385(18) 0.0436(19) 0.0456(19) -0.0033(15) 0.0118(15) 0.0139(15) C8C 0.0406(18) 0.0447(19) 0.049(2) -0.0085(15) 0.0007(15) 0.0217(16) C9C 0.0422(18) 0.0393(17) 0.0397(17) -0.0072(14) 0.0018(14) 0.0200(15) N10C 0.0285(13) 0.0468(16) 0.0365(14) 0.0108(12) 0.0096(11) 0.0139(12) C11C 0.0340(15) 0.0468(17) 0.0322(15) 0.0062(13) 0.0107(12) 0.0233(14) C12C 0.0365(16) 0.0504(19) 0.0307(15) 0.0060(13) 0.0109(12) 0.0225(15) O13C 0.0376(12) 0.0622(16) 0.0375(12) 0.0093(11) 0.0146(10) 0.0288(12) C14C 0.0475(19) 0.0518(19) 0.0264(15) 0.0071(13) 0.0108(13) 0.0265(16) C15C 0.0315(15) 0.0327(15) 0.0321(15) 0.0012(12) 0.0057(12) 0.0079(12) C16C 0.0308(14) 0.0267(14) 0.0355(15) 0.0031(12) 0.0040(12) 0.0044(12) C17C 0.0272(14) 0.0335(15) 0.0426(17) 0.0084(13) 0.0052(12) 0.0070(12) C18C 0.0329(15) 0.0333(16) 0.0484(19) 0.0039(14) 0.0079(14) 0.0097(13) C19C 0.0410(19) 0.054(2) 0.052(2) 0.0154(18) -0.0022(16) 0.0142(17) C20C 0.0431(19) 0.047(2) 0.0395(18) 0.0148(15) 0.0027(14) 0.0105(16) C21C 0.0337(16) 0.0379(17) 0.0360(16) 0.0055(13) 0.0024(13) 0.0037(13) N22C 0.061(2) 0.086(3) 0.061(2) 0.039(2) 0.0030(19) 0.015(2) O23C 0.067(2) 0.117(3) 0.067(2) 0.059(2) 0.0135(18) 0.016(2) O24C 0.091(3) 0.142(4) 0.083(3) 0.066(3) 0.010(2) 0.053(3) N25C 0.0353(16) 0.0527(19) 0.067(2) 0.0060(17) 0.0069(15) 0.0188(15) O26C 0.0554(19) 0.082(3) 0.111(3) 0.044(2) 0.050(2) 0.0389(19) O27C 0.0543(19) 0.114(3) 0.073(2) 0.018(2) 0.0062(16) 0.056(2) O28C 0.0529(15) 0.0447(14) 0.0353(12) 0.0051(10) 0.0031(11) 0.0244(12) C29C 0.062(2) 0.050(2) 0.0374(18) 0.0148(16) 0.0107(16) 0.0278(19) C30C 0.054(2) 0.082(3) 0.038(2) 0.018(2) 0.0072(17) 0.019(2) C31C 0.101(6) 0.079(5) 0.056(4) -0.011(3) 0.008(4) 0.042(4) C32C 0.069(4) 0.078(5) 0.062(4) 0.001(3) 0.009(3) 0.038(3) Si1C 0.0548(19) 0.0697(10) 0.048(2) -0.0058(16) 0.0193(15) 0.0326(14) C33C 0.070(4) 0.102(5) 0.066(4) 0.011(3) 0.029(3) 0.053(3) C34C 0.084(5) 0.095(5) 0.095(6) 0.016(4) 0.046(5) 0.056(5) C35C 0.129(8) 0.132(8) 0.065(4) 0.029(4) 0.041(5) 0.076(6) C36C 0.053(4) 0.114(6) 0.099(6) 0.010(5) 0.011(4) 0.039(4) C31G 0.101(6) 0.079(5) 0.056(4) -0.011(3) 0.008(4) 0.042(4) C32G 0.069(4) 0.078(5) 0.062(4) 0.001(3) 0.009(3) 0.038(3) Si1G 0.0548(19) 0.0697(10) 0.048(2) -0.0058(16) 0.0193(15) 0.0326(14) C33G 0.070(4) 0.102(5) 0.066(4) 0.011(3) 0.029(3) 0.053(3) C34G 0.084(5) 0.095(5) 0.095(6) 0.016(4) 0.046(5) 0.056(5) C35G 0.129(8) 0.132(8) 0.065(4) 0.029(4) 0.041(5) 0.076(6) C36G 0.053(4) 0.114(6) 0.099(6) 0.010(5) 0.011(4) 0.039(4) S1C 0.0483(6) 0.0355(5) 0.0399(5) 0.0029(4) -0.0037(5) 0.0178(5) O43C 0.0506(17) 0.0424(16) 0.0556(18) 0.0056(13) -0.0053(14) 0.0133(13) O44C 0.0537(19) 0.0458(15) 0.0629(19) 0.0067(13) -0.0079(16) 0.0240(14) C37C 0.061(2) 0.0340(17) 0.0361(18) 0.0068(14) -0.0042(16) 0.0146(16) C38C 0.060(2) 0.063(3) 0.0331(19) 0.0126(18) -0.0121(17) 0.011(2) C39C 0.083(3) 0.047(2) 0.051(3) 0.013(2) -0.009(2) -0.003(2) C40C 0.122(5) 0.044(3) 0.068(3) 0.002(2) 0.006(3) 0.013(3) C41C 0.111(4) 0.049(3) 0.095(4) -0.003(3) 0.029(4) 0.029(3) C42C 0.075(3) 0.045(2) 0.068(3) -0.001(2) 0.004(2) 0.026(2) S1G 0.0483(6) 0.0355(5) 0.0399(5) 0.0029(4) -0.0037(5) 0.0178(5) O43G 0.0506(17) 0.0424(16) 0.0556(18) 0.0056(13) -0.0053(14) 0.0133(13) O44G 0.0537(19) 0.0458(15) 0.0629(19) 0.0067(13) -0.0079(16) 0.0240(14) C37G 0.061(2) 0.0340(17) 0.0361(18) 0.0068(14) -0.0042(16) 0.0146(16) C38G 0.060(2) 0.063(3) 0.0331(19) 0.0126(18) -0.0121(17) 0.011(2) C39G 0.083(3) 0.047(2) 0.051(3) 0.013(2) -0.009(2) -0.003(2) C40G 0.122(5) 0.044(3) 0.068(3) 0.002(2) 0.006(3) 0.013(3) C41G 0.111(4) 0.049(3) 0.095(4) -0.003(3) 0.029(4) 0.029(3) C42G 0.075(3) 0.045(2) 0.068(3) -0.001(2) 0.004(2) 0.026(2) O45C 0.0421(14) 0.0588(17) 0.0512(15) 0.0237(13) 0.0051(12) 0.0169(13) O46C 0.0291(11) 0.0498(15) 0.0497(14) 0.0148(12) 0.0097(10) 0.0103(11) S1D 0.0461(5) 0.0430(5) 0.0579(6) 0.0104(4) 0.0094(4) 0.0117(4) N1D 0.0411(16) 0.0480(18) 0.0545(18) 0.0022(14) 0.0095(14) 0.0197(14) C2D 0.0359(17) 0.046(2) 0.051(2) -0.0145(16) 0.0002(15) 0.0127(15) C3D 0.0325(16) 0.045(2) 0.050(2) -0.0174(16) 0.0060(14) 0.0062(14) C4D 0.0375(17) 0.0372(17) 0.052(2) -0.0056(15) 0.0132(15) 0.0073(14) C5D 0.052(2) 0.046(2) 0.059(2) 0.0058(18) 0.0172(19) 0.0120(18) C6D 0.068(3) 0.071(3) 0.065(3) 0.020(2) 0.018(2) 0.035(3) C7D 0.057(3) 0.090(4) 0.073(3) 0.023(3) 0.023(2) 0.045(3) C8D 0.045(2) 0.067(3) 0.075(3) 0.022(2) 0.021(2) 0.028(2) C9D 0.0366(17) 0.0441(19) 0.057(2) 0.0047(16) 0.0102(15) 0.0157(15) C11D 0.0356(18) 0.058(2) 0.046(2) -0.0198(17) 0.0096(15) 0.0031(16) C12D 0.0310(16) 0.053(2) 0.056(2) -0.0261(18) 0.0068(15) 0.0016(15) O13D 0.0313(12) 0.0701(19) 0.0604(18) -0.0335(15) 0.0023(12) 0.0100(12) C14D 0.0297(16) 0.064(2) 0.0423(19) -0.0218(16) -0.0047(14) 0.0103(16) N10D 0.030(3) 0.051(4) 0.035(4) -0.009(2) -0.004(3) 0.015(2) C15D 0.041(4) 0.033(4) 0.043(4) -0.008(2) 0.001(3) 0.008(2) O46D 0.040(4) 0.052(3) 0.056(4) 0.005(3) -0.002(3) 0.016(2) C16D 0.051(4) 0.033(5) 0.069(6) -0.005(3) 0.014(4) 0.015(3) C17D 0.064(5) 0.032(4) 0.056(5) -0.009(3) 0.011(4) 0.009(4) C18D 0.063(5) 0.028(3) 0.063(5) -0.012(3) 0.015(4) 0.001(3) C19D 0.061(4) 0.029(4) 0.072(6) -0.012(3) 0.018(4) -0.008(3) C20D 0.056(4) 0.035(6) 0.063(6) -0.006(4) 0.021(4) -0.001(3) C21D 0.048(4) 0.032(4) 0.054(4) -0.014(3) 0.009(3) 0.003(3) N22D 0.055(4) 0.053(5) 0.068(4) -0.011(3) 0.019(3) -0.001(3) O23D 0.072(5) 0.079(6) 0.089(6) 0.001(4) 0.048(4) 0.006(4) O24D 0.061(4) 0.094(7) 0.077(6) 0.004(5) 0.028(4) 0.026(4) N25D 0.092(7) 0.024(4) 0.084(7) 0.002(4) 0.015(5) -0.004(5) O26D 0.131(7) 0.048(3) 0.060(4) 0.006(3) 0.014(4) 0.027(4) O27D 0.095(6) 0.074(5) 0.103(7) 0.021(5) -0.003(5) 0.015(5) N10H 0.030(3) 0.051(4) 0.035(4) -0.009(2) -0.004(3) 0.015(2) C15H 0.041(4) 0.033(4) 0.043(4) -0.008(2) 0.001(3) 0.008(2) O46H 0.040(4) 0.052(3) 0.056(4) 0.005(3) -0.002(3) 0.016(2) C16H 0.063(6) 0.026(5) 0.060(6) -0.010(4) 0.018(5) -0.002(5) C17H 0.072(7) 0.031(6) 0.054(7) -0.005(4) 0.004(6) -0.022(5) C18H 0.093(8) 0.032(5) 0.054(6) -0.001(4) 0.015(6) -0.014(5) C19H 0.102(8) 0.029(7) 0.076(10) 0.000(5) 0.050(7) 0.001(6) C20H 0.084(6) 0.040(6) 0.081(8) 0.002(5) 0.048(6) 0.007(5) C21H 0.061(6) 0.034(6) 0.076(8) 0.004(5) 0.033(6) 0.000(4) N22H 0.069(7) 0.077(10) 0.099(11) 0.003(8) 0.055(8) 0.009(6) O23H 0.131(10) 0.078(7) 0.181(15) 0.037(8) 0.128(11) 0.040(7) O24H 0.072(7) 0.130(12) 0.209(16) 0.084(11) 0.084(9) 0.041(7) N25H 0.123(9) 0.050(7) 0.070(8) 0.017(5) 0.013(7) -0.012(7) O26H 0.173(11) 0.037(4) 0.062(6) 0.008(4) 0.036(7) 0.013(6) O27H 0.103(9) 0.072(9) 0.104(11) 0.043(8) -0.034(8) -0.045(8) O28D 0.0299(12) 0.0529(15) 0.0559(16) -0.0209(12) 0.0021(11) 0.0094(11) C29D 0.050(2) 0.058(2) 0.056(2) -0.0165(19) -0.0022(19) 0.016(2) C30D 0.108(5) 0.100(5) 0.060(3) 0.002(3) 0.005(3) 0.062(4) C31D 0.043(5) 0.078(5) 0.089(4) -0.029(4) 0.015(4) -0.005(3) C32D 0.063(8) 0.111(6) 0.082(4) -0.001(4) -0.031(4) 0.021(6) Si1D 0.044(3) 0.062(4) 0.190(6) 0.046(4) -0.037(3) -0.021(2) C33D 0.030(3) 0.153(7) 0.105(6) 0.013(5) 0.012(3) 0.031(4) C34D 0.141(9) 0.135(7) 0.094(7) 0.007(5) 0.009(6) 0.092(7) C35D 0.051(4) 0.222(12) 0.109(8) 0.006(8) -0.037(6) 0.021(6) C36D 0.071(6) 0.154(10) 0.104(6) 0.001(6) 0.024(5) 0.011(6) C31H 0.043(5) 0.078(5) 0.089(4) -0.029(4) 0.015(4) -0.005(3) C32H 0.063(8) 0.111(6) 0.082(4) -0.001(4) -0.031(4) 0.021(6) Si1H 0.0402(13) 0.0515(19) 0.110(2) -0.0445(17) -0.0210(15) 0.0131(15) C33H 0.030(3) 0.153(7) 0.105(6) 0.013(5) 0.012(3) 0.031(4) C34H 0.141(9) 0.135(7) 0.094(7) 0.007(5) 0.009(6) 0.092(7) C35H 0.051(4) 0.222(12) 0.109(8) 0.006(8) -0.037(6) 0.021(6) C36H 0.071(6) 0.154(10) 0.104(6) 0.001(6) 0.024(5) 0.011(6) C37D 0.057(2) 0.0437(18) 0.0408(18) 0.0142(15) 0.0227(16) 0.0202(16) C38D 0.065(2) 0.0410(19) 0.043(2) 0.0099(15) 0.0089(17) 0.0201(18) C39D 0.085(3) 0.041(2) 0.049(2) 0.0068(17) 0.004(2) 0.019(2) C40D 0.107(4) 0.044(2) 0.048(2) 0.0024(18) 0.019(2) 0.033(2) C41D 0.093(4) 0.055(3) 0.084(4) 0.012(2) 0.042(3) 0.043(3) C42D 0.069(3) 0.067(3) 0.080(3) 0.021(2) 0.031(2) 0.037(2) O43D 0.0526(18) 0.074(2) 0.082(2) 0.032(2) 0.0180(17) 0.0091(16) O44D 0.066(2) 0.0359(14) 0.073(2) 0.0045(14) -0.0055(16) 0.0109(13) O45D 0.0438(15) 0.087(2) 0.0445(15) -0.0188(15) 0.0044(12) 0.0307(16) Cl1S 0.0601(11) 0.0683(12) 0.0924(15) 0.0069(10) -0.0073(9) 0.0269(9) Cl2S 0.124(2) 0.0674(12) 0.0625(12) 0.0129(9) 0.0176(12) 0.0150(12) C1S 0.109(7) 0.076(5) 0.053(4) 0.010(3) -0.019(4) 0.039(5) Cl3S 0.117(3) 0.166(4) 0.139(3) 0.062(3) 0.066(2) 0.082(3) Cl4S 0.179(4) 0.155(4) 0.139(3) 0.029(3) 0.070(3) 0.115(4) C2S 0.124(10) 0.119(8) 0.123(10) 0.008(8) 0.017(8) 0.081(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1A O43A 1.411(3) . ? S1A O44A 1.431(4) . ? S1A N1A 1.676(4) . ? S1A C37A 1.751(4) . ? N1A C9A 1.394(5) . ? N1A C2A 1.418(5) . ? C2A C3A 1.368(6) . ? C3A C4A 1.448(5) . ? C3A C12A 1.505(5) . ? C4A C5A 1.389(6) . ? C4A C9A 1.409(5) . ? C5A C6A 1.389(5) . ? C6A C7A 1.402(6) . ? C7A C8A 1.374(7) . ? C8A C9A 1.394(5) . ? N10A C15A 1.359(5) . ? N10A C11A 1.445(5) . ? C11A C14A 1.499(6) . ? C11A C12A 1.547(5) . ? C12A O13A 1.414(5) . ? O13A Si1A 1.655(3) . ? O13A Si1E 1.764(6) . ? C14A O45A 1.198(5) . ? C14A O28A 1.345(5) . ? C15A O46A 1.221(4) . ? C15A C16A 1.492(6) . ? C16A C17A 1.389(5) . ? C16A C21A 1.401(6) . ? C17A C18A 1.356(6) . ? C18A C19A 1.389(6) . ? C18A N25A 1.478(6) . ? C19A C20A 1.386(6) . ? C20A C21A 1.367(6) . ? C20A N22A 1.471(6) . ? N22A O23A 1.212(6) . ? N22A O24A 1.223(6) . ? N25A O27A 1.199(6) . ? N25A O26A 1.220(7) . ? O28A C29A 1.446(6) . ? C29A C30E 1.516(11) . ? C29A C30A 1.528(15) . ? Si1A C32A 1.850(7) . ? Si1A C31A 1.869(7) . ? Si1A C33A 1.885(10) . ? C33A C36A 1.538(10) . ? C33A C35A 1.549(9) . ? C33A C34A 1.559(11) . ? Si1E C31E 1.810(13) . ? Si1E C32E 1.859(14) . ? Si1E C33E 1.860(16) . ? C33E C35E 1.544(14) . ? C33E C34E 1.550(15) . ? C33E C36E 1.553(14) . ? C37A C42A 1.365(8) . ? C37A C38A 1.421(7) . ? C38A C39A 1.366(8) . ? C39A C40A 1.412(10) . ? C40A C41A 1.302(9) . ? C41A C42A 1.414(7) . ? Si1B O13B 1.654(3) . ? Si1B C32B 1.863(5) . ? Si1B C33B 1.868(5) . ? Si1B C31B 1.870(6) . ? S1B O44B 1.266(4) . ? S1B O43B 1.399(4) . ? S1B N1B 1.650(4) . ? S1B C37B 1.758(5) . ? N1B C2B 1.390(6) . ? N1B C9B 1.419(6) . ? C2B C3B 1.349(6) . ? C3B C4B 1.449(5) . ? C3B C12B 1.481(6) . ? C4B C9B 1.380(6) . ? C4B C5B 1.418(6) . ? C5B C6B 1.390(5) . ? C6B C7B 1.374(7) . ? C7B C8B 1.391(8) . ? C8B C9B 1.392(7) . ? N10B C15B 1.328(6) . ? N10B C11B 1.448(6) . ? C11B C14B 1.513(6) . ? C11B C12B 1.548(6) . ? C12B O13B 1.421(5) . ? C14B O45B 1.198(6) . ? C14B O28B 1.322(6) . ? C15B O46B 1.236(5) . ? C15B C16B 1.488(7) . ? C16B C21B 1.392(6) . ? C16B C17B 1.403(6) . ? C17B C18B 1.368(7) . ? C18B C19B 1.394(7) . ? C18B N25B 1.481(6) . ? C19B C20B 1.392(7) . ? C20B C21B 1.379(7) . ? C20B N22B 1.479(7) . ? N22B O23B 1.205(6) . ? N22B O24B 1.223(6) . ? N25B O27B 1.221(6) . ? N25B O26B 1.248(7) . ? O28B C29B 1.463(7) . ? C29B C30F 1.318(19) . ? C29B C30B 1.325(12) . ? C33B C35B 1.533(7) . ? C33B C36B 1.535(7) . ? C33B C34B 1.542(6) . ? C37B C38B 1.374(7) . ? C37B C42B 1.375(8) . ? C38B C39B 1.441(8) . ? C39B C40B 1.375(9) . ? C40B C41B 1.390(8) . ? C41B C42B 1.378(8) . ? N1C C9C 1.402(5) . ? N1C C2C 1.402(5) . ? N1C S1C 1.659(4) . ? N1C S1G 2.058(16) . ? C2C C3C 1.332(6) . ? C3C C4C 1.449(5) . ? C3C C12C 1.519(5) . ? C4C C5C 1.398(5) . ? C4C C9C 1.419(5) . ? C5C C6C 1.383(5) . ? C7C C8C 1.375(7) . ? C7C C6C 1.414(6) . ? C8C C9C 1.392(5) . ? N10C C15C 1.343(5) . ? N10C C11C 1.450(4) . ? C11C C14C 1.527(5) . ? C11C C12C 1.540(5) . ? C12C O13C 1.414(4) . ? O13C Si1C 1.623(5) . ? O13C Si1G 1.706(7) . ? C14C O45C 1.202(5) . ? C14C O28C 1.322(4) . ? C15C O46C 1.213(4) . ? C15C C16C 1.521(5) . ? C16C C21C 1.379(5) . ? C16C C17C 1.409(5) . ? C17C C18C 1.375(5) . ? C18C C19C 1.378(6) . ? C18C N25C 1.474(5) . ? C19C C20C 1.391(6) . ? C20C C21C 1.381(5) . ? C20C N22C 1.455(5) . ? N22C O24C 1.214(6) . ? N22C O23C 1.235(6) . ? N25C O27C 1.190(5) . ? N25C O26C 1.223(6) . ? O28C C29C 1.460(5) . ? C29C C30C 1.512(6) . ? C31C Si1C 1.948(11) . ? C32C Si1C 1.836(9) . ? Si1C C33C 1.821(10) . ? C33C C35C 1.513(11) . ? C33C C34C 1.564(9) . ? C33C C36C 1.597(11) . ? C31G Si1G 1.815(11) . ? C32G Si1G 1.881(11) . ? Si1G C33G 1.859(12) . ? C33G C36G 1.534(12) . ? C33G C34G 1.553(12) . ? C33G C35G 1.560(11) . ? S1C O44C 1.407(4) . ? S1C O43C 1.441(4) . ? S1C C37C 1.748(4) . ? C37C C42C 1.379(7) . ? C37C C38C 1.380(6) . ? C38C C39C 1.425(7) . ? C39C C40C 1.337(9) . ? C40C C41C 1.381(9) . ? C41C C42C 1.402(7) . ? S1G O44G 1.420(17) . ? S1G O43G 1.436(16) . ? S1G C37G 1.743(17) . ? C37G C38G 1.373(16) . ? C37G C42G 1.394(16) . ? C38G C39G 1.433(17) . ? C39G C40G 1.352(17) . ? C40G C41G 1.359(17) . ? C41G C42G 1.413(17) . ? S1D O44D 1.422(4) . ? S1D O43D 1.431(4) . ? S1D N1D 1.650(4) . ? S1D C37D 1.769(4) . ? N1D C2D 1.409(5) . ? N1D C9D 1.423(6) . ? C2D C3D 1.360(7) . ? C3D C4D 1.422(6) . ? C3D C12D 1.504(5) . ? C4D C9D 1.401(6) . ? C4D C5D 1.415(7) . ? C5D C6D 1.383(7) . ? C6D C7D 1.411(7) . ? C7D C8D 1.383(8) . ? C8D C9D 1.394(6) . ? C11D N10H 1.396(14) . ? C11D C14D 1.511(7) . ? C11D C12D 1.545(5) . ? C11D N10D 1.547(10) . ? C12D O13D 1.400(6) . ? O13D Si1D 1.605(7) . ? O13D Si1H 1.701(5) . ? C14D O45D 1.205(5) . ? C14D O28D 1.319(6) . ? N10D C15D 1.377(10) . ? C15D O46D 1.206(9) . ? C15D C16D 1.522(10) . ? C16D C21D 1.375(10) . ? C16D C17D 1.382(11) . ? C17D C18D 1.396(10) . ? C18D C19D 1.350(11) . ? C18D N25D 1.458(15) . ? C19D C20D 1.381(12) . ? C20D C21D 1.403(10) . ? C20D N22D 1.475(12) . ? N22D O23D 1.209(9) . ? N22D O24D 1.234(11) . ? N25D O26D 1.207(10) . ? N25D O27D 1.243(12) . ? N10H C15H 1.373(13) . ? C15H O46H 1.214(12) . ? C15H C16H 1.500(13) . ? C16H C21H 1.362(13) . ? C16H C17H 1.381(13) . ? C17H C18H 1.405(13) . ? C18H C19H 1.358(14) . ? C18H N25H 1.462(16) . ? C19H C20H 1.346(14) . ? C20H C21H 1.403(12) . ? C20H N22H 1.490(17) . ? N22H O24H 1.211(13) . ? N22H O23H 1.222(12) . ? N25H O26H 1.220(12) . ? N25H O27H 1.223(13) . ? O28D C29D 1.468(6) . ? C29D C30D 1.456(8) . ? C31D Si1D 1.799(14) . ? C32D Si1D 2.116(14) . ? Si1D C33D 1.802(14) . ? C33D C34D 1.556(14) . ? C33D C35D 1.567(13) . ? C33D C36D 1.580(13) . ? C31H Si1H 1.818(12) . ? C32H Si1H 1.984(11) . ? Si1H C33H 1.871(10) . ? C33H C36H 1.539(12) . ? C33H C34H 1.540(13) . ? C33H C35H 1.563(11) . ? C37D C38D 1.374(6) . ? C37D C42D 1.390(6) . ? C38D C39D 1.386(6) . ? C39D C40D 1.373(8) . ? C40D C41D 1.345(9) . ? C41D C42D 1.409(9) . ? Cl1S C1S 1.704(9) . ? Cl2S C1S 1.733(9) . ? Cl3S C2S 1.718(18) . ? Cl4S C2S 1.753(12) . ? 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 O43A S1A O44A 121.7(2) . . ? O43A S1A N1A 105.6(2) . . ? O44A S1A N1A 105.8(2) . . ? O43A S1A C37A 107.9(2) . . ? O44A S1A C37A 109.6(2) . . ? N1A S1A C37A 105.0(2) . . ? C9A N1A C2A 108.6(3) . . ? C9A N1A S1A 125.8(3) . . ? C2A N1A S1A 123.8(3) . . ? C3A C2A N1A 108.6(3) . . ? C2A C3A C4A 107.8(3) . . ? C2A C3A C12A 125.9(3) . . ? C4A C3A C12A 126.2(4) . . ? C5A C4A C9A 119.5(3) . . ? C5A C4A C3A 133.3(4) . . ? C9A C4A C3A 107.2(3) . . ? C6A C5A C4A 118.6(4) . . ? C5A C6A C7A 120.8(4) . . ? C8A C7A C6A 121.6(4) . . ? C7A C8A C9A 117.3(4) . . ? N1A C9A C8A 130.2(4) . . ? N1A C9A C4A 107.8(3) . . ? C8A C9A C4A 122.0(4) . . ? C15A N10A C11A 120.4(3) . . ? N10A C11A C14A 107.8(3) . . ? N10A C11A C12A 110.5(3) . . ? C14A C11A C12A 110.6(3) . . ? O13A C12A C3A 110.1(4) . . ? O13A C12A C11A 108.3(3) . . ? C3A C12A C11A 112.3(3) . . ? C12A O13A Si1A 131.4(3) . . ? C12A O13A Si1E 120.4(4) . . ? Si1A O13A Si1E 19.24(17) . . ? O45A C14A O28A 124.9(4) . . ? O45A C14A C11A 124.6(4) . . ? O28A C14A C11A 110.5(3) . . ? O46A C15A N10A 121.6(4) . . ? O46A C15A C16A 121.5(4) . . ? N10A C15A C16A 116.8(3) . . ? C17A C16A C21A 119.2(4) . . ? C17A C16A C15A 123.6(4) . . ? C21A C16A C15A 117.2(3) . . ? C18A C17A C16A 119.3(4) . . ? C17A C18A C19A 123.6(4) . . ? C17A C18A N25A 118.7(4) . . ? C19A C18A N25A 117.8(4) . . ? C20A C19A C18A 115.7(4) . . ? C21A C20A C19A 123.2(4) . . ? C21A C20A N22A 118.7(4) . . ? C19A C20A N22A 117.9(4) . . ? C20A C21A C16A 119.0(4) . . ? O23A N22A O24A 123.8(4) . . ? O23A N22A C20A 118.3(4) . . ? O24A N22A C20A 117.9(4) . . ? O27A N25A O26A 124.1(4) . . ? O27A N25A C18A 119.6(4) . . ? O26A N25A C18A 116.2(4) . . ? C14A O28A C29A 117.6(4) . . ? O28A C29A C30E 113.3(6) . . ? O28A C29A C30A 107.0(8) . . ? C30E C29A C30A 42.0(9) . . ? O13A Si1A C32A 113.4(3) . . ? O13A Si1A C31A 107.5(3) . . ? C32A Si1A C31A 108.9(5) . . ? O13A Si1A C33A 103.9(3) . . ? C32A Si1A C33A 109.0(5) . . ? C31A Si1A C33A 114.2(4) . . ? C36A C33A C35A 107.5(7) . . ? C36A C33A C34A 108.3(9) . . ? C35A C33A C34A 110.0(7) . . ? C36A C33A Si1A 110.8(6) . . ? C35A C33A Si1A 110.9(7) . . ? C34A C33A Si1A 109.4(6) . . ? O13A Si1E C31E 115.7(6) . . ? O13A Si1E C32E 108.4(7) . . ? C31E Si1E C32E 109.8(11) . . ? O13A Si1E C33E 97.0(7) . . ? C31E Si1E C33E 115.2(10) . . ? C32E Si1E C33E 110.1(11) . . ? C35E C33E C34E 109.0(16) . . ? C35E C33E C36E 111.7(15) . . ? C34E C33E C36E 109.8(16) . . ? C35E C33E Si1E 112.2(13) . . ? C34E C33E Si1E 106.3(14) . . ? C36E C33E Si1E 107.7(14) . . ? C42A C37A C38A 119.0(5) . . ? C42A C37A S1A 120.8(4) . . ? C38A C37A S1A 120.2(4) . . ? C39A C38A C37A 120.4(6) . . ? C38A C39A C40A 118.7(6) . . ? C41A C40A C39A 121.0(5) . . ? C40A C41A C42A 121.8(6) . . ? C37A C42A C41A 119.0(6) . . ? O13B Si1B C32B 109.3(2) . . ? O13B Si1B C33B 102.37(17) . . ? C32B Si1B C33B 113.4(2) . . ? O13B Si1B C31B 111.1(2) . . ? C32B Si1B C31B 109.7(3) . . ? C33B Si1B C31B 110.8(3) . . ? O44B S1B O43B 118.5(3) . . ? O44B S1B N1B 102.2(2) . . ? O43B S1B N1B 107.7(2) . . ? O44B S1B C37B 113.3(2) . . ? O43B S1B C37B 109.0(3) . . ? N1B S1B C37B 104.8(2) . . ? C2B N1B C9B 109.0(4) . . ? C2B N1B S1B 121.1(3) . . ? C9B N1B S1B 128.1(3) . . ? C3B C2B N1B 109.4(4) . . ? C2B C3B C4B 106.9(4) . . ? C2B C3B C12B 126.5(4) . . ? C4B C3B C12B 126.6(4) . . ? C9B C4B C5B 119.0(4) . . ? C9B C4B C3B 108.9(4) . . ? C5B C4B C3B 132.1(4) . . ? C6B C5B C4B 118.1(4) . . ? C7B C6B C5B 121.5(4) . . ? C6B C7B C8B 121.3(4) . . ? C7B C8B C9B 117.1(4) . . ? C4B C9B C8B 122.9(5) . . ? C4B C9B N1B 105.8(4) . . ? C8B C9B N1B 131.3(4) . . ? C15B N10B C11B 120.6(3) . . ? N10B C11B C14B 107.4(3) . . ? N10B C11B C12B 110.6(3) . . ? C14B C11B C12B 112.2(4) . . ? O13B C12B C3B 110.7(3) . . ? O13B C12B C11B 107.1(3) . . ? C3B C12B C11B 113.3(3) . . ? C12B O13B Si1B 125.9(2) . . ? O45B C14B O28B 126.9(5) . . ? O45B C14B C11B 123.5(5) . . ? O28B C14B C11B 109.6(4) . . ? O46B C15B N10B 121.7(4) . . ? O46B C15B C16B 121.8(4) . . ? N10B C15B C16B 116.5(3) . . ? C21B C16B C17B 120.1(4) . . ? C21B C16B C15B 117.3(4) . . ? C17B C16B C15B 122.6(4) . . ? C18B C17B C16B 118.9(4) . . ? C17B C18B C19B 123.1(4) . . ? C17B C18B N25B 118.4(4) . . ? C19B C18B N25B 118.5(4) . . ? C20B C19B C18B 116.2(4) . . ? C21B C20B C19B 123.1(5) . . ? C21B C20B N22B 117.8(4) . . ? C19B C20B N22B 119.0(5) . . ? C20B C21B C16B 118.6(4) . . ? O23B N22B O24B 124.3(5) . . ? O23B N22B C20B 118.4(4) . . ? O24B N22B C20B 117.3(5) . . ? O27B N25B O26B 124.9(4) . . ? O27B N25B C18B 118.8(5) . . ? O26B N25B C18B 116.3(4) . . ? C14B O28B C29B 114.9(5) . . ? C30F C29B C30B 122.9(13) . . ? C30F C29B O28B 116.8(12) . . ? C30B C29B O28B 108.5(6) . . ? C35B C33B C36B 108.9(5) . . ? C35B C33B C34B 109.4(4) . . ? C36B C33B C34B 108.7(4) . . ? C35B C33B Si1B 110.1(3) . . ? C36B C33B Si1B 109.3(4) . . ? C34B C33B Si1B 110.4(4) . . ? C38B C37B C42B 123.9(5) . . ? C38B C37B S1B 116.5(4) . . ? C42B C37B S1B 119.5(4) . . ? C37B C38B C39B 115.8(5) . . ? C40B C39B C38B 120.3(5) . . ? C39B C40B C41B 121.1(5) . . ? C42B C41B C40B 119.2(6) . . ? C37B C42B C41B 119.6(5) . . ? C9C N1C C2C 108.6(3) . . ? C9C N1C S1C 126.4(3) . . ? C2C N1C S1C 122.8(3) . . ? C9C N1C S1G 114.2(5) . . ? C2C N1C S1G 129.6(5) . . ? S1C N1C S1G 15.4(4) . . ? C3C C2C N1C 110.3(3) . . ? C2C C3C C4C 107.4(3) . . ? C2C C3C C12C 126.5(3) . . ? C4C C3C C12C 126.0(3) . . ? C5C C4C C9C 118.9(3) . . ? C5C C4C C3C 133.6(3) . . ? C9C C4C C3C 107.5(3) . . ? C6C C5C C4C 119.3(4) . . ? C8C C7C C6C 122.1(4) . . ? C5C C6C C7C 120.2(4) . . ? C7C C8C C9C 117.1(4) . . ? C8C C9C N1C 131.5(4) . . ? C8C C9C C4C 122.4(4) . . ? N1C C9C C4C 106.1(3) . . ? C15C N10C C11C 122.3(3) . . ? N10C C11C C14C 107.4(3) . . ? N10C C11C C12C 109.0(3) . . ? C14C C11C C12C 113.7(3) . . ? O13C C12C C3C 110.1(3) . . ? O13C C12C C11C 108.0(3) . . ? C3C C12C C11C 113.7(3) . . ? C12C O13C Si1C 129.2(3) . . ? C12C O13C Si1G 126.4(4) . . ? Si1C O13C Si1G 15.0(3) . . ? O45C C14C O28C 126.2(4) . . ? O45C C14C C11C 123.4(3) . . ? O28C C14C C11C 110.4(3) . . ? O46C C15C N10C 124.8(3) . . ? O46C C15C C16C 120.1(3) . . ? N10C C15C C16C 115.0(3) . . ? C21C C16C C17C 120.1(3) . . ? C21C C16C C15C 117.6(3) . . ? C17C C16C C15C 122.3(3) . . ? C18C C17C C16C 118.9(3) . . ? C17C C18C C19C 122.8(3) . . ? C17C C18C N25C 118.6(3) . . ? C19C C18C N25C 118.6(4) . . ? C18C C19C C20C 116.3(4) . . ? C21C C20C C19C 123.4(4) . . ? C21C C20C N22C 119.1(4) . . ? C19C C20C N22C 117.5(4) . . ? C16C C21C C20C 118.4(3) . . ? O24C N22C O23C 124.0(4) . . ? O24C N22C C20C 118.9(4) . . ? O23C N22C C20C 117.1(4) . . ? O27C N25C O26C 125.1(4) . . ? O27C N25C C18C 117.9(4) . . ? O26C N25C C18C 117.1(3) . . ? C14C O28C C29C 117.9(3) . . ? O28C C29C C30C 108.6(4) . . ? O13C Si1C C33C 107.8(4) . . ? O13C Si1C C32C 111.3(4) . . ? C33C Si1C C32C 115.7(5) . . ? O13C Si1C C31C 107.9(4) . . ? C33C Si1C C31C 107.8(5) . . ? C32C Si1C C31C 106.1(6) . . ? C35C C33C C34C 115.8(7) . . ? C35C C33C C36C 110.0(8) . . ? C34C C33C C36C 104.8(7) . . ? C35C C33C Si1C 108.0(7) . . ? C34C C33C Si1C 109.3(7) . . ? C36C C33C Si1C 108.8(6) . . ? O13C Si1G C31G 110.3(5) . . ? O13C Si1G C33G 106.5(4) . . ? C31G Si1G C33G 113.6(7) . . ? O13C Si1G C32G 103.8(5) . . ? C31G Si1G C32G 111.3(7) . . ? C33G Si1G C32G 110.8(5) . . ? C36G C33G C34G 111.5(9) . . ? C36G C33G C35G 110.7(8) . . ? C34G C33G C35G 107.8(8) . . ? C36G C33G Si1G 109.3(7) . . ? C34G C33G Si1G 108.8(7) . . ? C35G C33G Si1G 108.7(8) . . ? O44C S1C O43C 120.0(4) . . ? O44C S1C N1C 107.6(4) . . ? O43C S1C N1C 104.6(2) . . ? O44C S1C C37C 111.0(3) . . ? O43C S1C C37C 107.7(2) . . ? N1C S1C C37C 104.57(19) . . ? C42C C37C C38C 122.5(5) . . ? C42C C37C S1C 118.4(4) . . ? C38C C37C S1C 119.1(4) . . ? C37C C38C C39C 117.7(5) . . ? C40C C39C C38C 119.8(5) . . ? C39C C40C C41C 122.5(6) . . ? C40C C41C C42C 119.2(6) . . ? C37C C42C C41C 118.3(6) . . ? O44G S1G O43G 120(3) . . ? O44G S1G C37G 112(3) . . ? O43G S1G C37G 102.9(17) . . ? O44G S1G N1C 95(5) . . ? O43G S1G N1C 93.5(17) . . ? C37G S1G N1C 134.2(16) . . ? C38G C37G C42G 119(2) . . ? C38G C37G S1G 129(2) . . ? C42G C37G S1G 111.1(18) . . ? C37G C38G C39G 119.8(19) . . ? C40G C39G C38G 119(2) . . ? C39G C40G C41G 122(2) . . ? C40G C41G C42G 118(2) . . ? C37G C42G C41G 120(2) . . ? O44D S1D O43D 120.8(2) . . ? O44D S1D N1D 105.3(2) . . ? O43D S1D N1D 106.5(2) . . ? O44D S1D C37D 107.8(2) . . ? O43D S1D C37D 109.3(2) . . ? N1D S1D C37D 106.32(18) . . ? C2D N1D C9D 107.5(4) . . ? C2D N1D S1D 122.9(3) . . ? C9D N1D S1D 128.0(3) . . ? C3D C2D N1D 109.4(4) . . ? C2D C3D C4D 107.9(3) . . ? C2D C3D C12D 125.4(4) . . ? C4D C3D C12D 126.7(4) . . ? C9D C4D C5D 118.7(4) . . ? C9D C4D C3D 108.4(4) . . ? C5D C4D C3D 132.9(4) . . ? C6D C5D C4D 118.9(4) . . ? C5D C6D C7D 120.3(5) . . ? C8D C7D C6D 122.5(4) . . ? C7D C8D C9D 116.1(4) . . ? C8D C9D C4D 123.6(4) . . ? C8D C9D N1D 129.7(4) . . ? C4D C9D N1D 106.7(3) . . ? N10H C11D C14D 99.9(6) . . ? N10H C11D C12D 106.0(7) . . ? C14D C11D C12D 112.5(4) . . ? N10H C11D N10D 18.9(5) . . ? C14D C11D N10D 113.1(5) . . ? C12D C11D N10D 110.6(5) . . ? O13D C12D C3D 111.8(4) . . ? O13D C12D C11D 108.3(3) . . ? C3D C12D C11D 113.7(3) . . ? C12D O13D Si1D 135.9(4) . . ? C12D O13D Si1H 120.7(4) . . ? Si1D O13D Si1H 17.0(3) . . ? O45D C14D O28D 126.1(5) . . ? O45D C14D C11D 123.3(4) . . ? O28D C14D C11D 110.6(3) . . ? C15D N10D C11D 126.2(7) . . ? O46D C15D N10D 123.2(8) . . ? O46D C15D C16D 120.9(8) . . ? N10D C15D C16D 115.9(7) . . ? C21D C16D C17D 119.2(8) . . ? C21D C16D C15D 123.6(9) . . ? C17D C16D C15D 117.2(7) . . ? C16D C17D C18D 119.5(9) . . ? C19D C18D C17D 123.4(10) . . ? C19D C18D N25D 116.3(8) . . ? C17D C18D N25D 120.3(9) . . ? C18D C19D C20D 116.2(9) . . ? C19D C20D C21D 122.9(9) . . ? C19D C20D N22D 119.1(7) . . ? C21D C20D N22D 118.0(9) . . ? C16D C21D C20D 118.9(9) . . ? O23D N22D O24D 123.8(10) . . ? O23D N22D C20D 118.1(9) . . ? O24D N22D C20D 118.0(8) . . ? O26D N25D O27D 122.7(12) . . ? O26D N25D C18D 119.8(10) . . ? O27D N25D C18D 117.3(8) . . ? C15H N10H C11D 111.3(10) . . ? O46H C15H N10H 123.5(11) . . ? O46H C15H C16H 121.1(13) . . ? N10H C15H C16H 115.2(11) . . ? C21H C16H C17H 121.0(11) . . ? C21H C16H C15H 122.2(10) . . ? C17H C16H C15H 116.8(10) . . ? C16H C17H C18H 118.3(13) . . ? C19H C18H C17H 121.9(13) . . ? C19H C18H N25H 118.9(10) . . ? C17H C18H N25H 119.1(12) . . ? C20H C19H C18H 117.7(12) . . ? C19H C20H C21H 123.4(13) . . ? C19H C20H N22H 119.1(10) . . ? C21H C20H N22H 117.4(11) . . ? C16H C21H C20H 117.7(12) . . ? O24H N22H O23H 124.7(16) . . ? O24H N22H C20H 118.0(10) . . ? O23H N22H C20H 116.4(12) . . ? O26H N25H O27H 123.1(16) . . ? O26H N25H C18H 119.0(12) . . ? O27H N25H C18H 117.8(11) . . ? C14D O28D C29D 118.2(3) . . ? C30D C29D O28D 108.5(4) . . ? O13D Si1D C31D 109.8(7) . . ? O13D Si1D C33D 121.3(6) . . ? C31D Si1D C33D 118.5(8) . . ? O13D Si1D C32D 95.7(7) . . ? C31D Si1D C32D 103.6(10) . . ? C33D Si1D C32D 103.0(8) . . ? C34D C33D C35D 105.5(13) . . ? C34D C33D C36D 121.0(13) . . ? C35D C33D C36D 118.1(12) . . ? C34D C33D Si1D 105.6(8) . . ? C35D C33D Si1D 105.4(10) . . ? C36D C33D Si1D 99.2(9) . . ? O13D Si1H C31H 111.7(5) . . ? O13D Si1H C33H 104.5(4) . . ? C31H Si1H C33H 98.3(6) . . ? O13D Si1H C32H 107.2(6) . . ? C31H Si1H C32H 121.1(7) . . ? C33H Si1H C32H 112.7(6) . . ? C36H C33H C34H 106.5(11) . . ? C36H C33H C35H 109.4(9) . . ? C34H C33H C35H 110.0(11) . . ? C36H C33H Si1H 115.2(9) . . ? C34H C33H Si1H 109.1(8) . . ? C35H C33H Si1H 106.7(9) . . ? C38D C37D C42D 121.4(4) . . ? C38D C37D S1D 119.4(3) . . ? C42D C37D S1D 119.1(4) . . ? C37D C38D C39D 119.4(4) . . ? C40D C39D C38D 120.0(5) . . ? C41D C40D C39D 120.6(5) . . ? C40D C41D C42D 121.5(5) . . ? C37D C42D C41D 117.1(5) . . ? Cl1S C1S Cl2S 116.2(5) . . ? Cl3S C2S Cl4S 109.2(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.234 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.072 _database_code_depnum_ccdc_archive 'CCDC 933936' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_x8_12224 #TrackingRef 'X8_12224-triacetate.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H50 N4 O14 S' _chemical_formula_weight 902.95 _chemical_absolute_configuration ad 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.8803(7) _cell_length_b 10.3954(6) _cell_length_c 16.5478(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.0630(10) _cell_angle_gamma 90.00 _cell_volume 2215.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9973 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 31.61 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9373 _exptl_absorpt_correction_T_max 0.9771 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. Please acknowledge this grant in all publications of this structure. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 179249 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0136 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 30.51 _reflns_number_total 13500 _reflns_number_gt 13130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0541P)^2^+0.3809P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 13500 _refine_ls_number_parameters 588 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 N1 N -0.11813(7) -0.88033(9) -0.19631(5) 0.01520(16) Uani 1 1 d . . . C2 C -0.07862(7) -0.75113(10) -0.21925(6) 0.01392(17) Uani 1 1 d . . . H2 H -0.0535 -0.7030 -0.1707 0.017 Uiso 1 1 calc R . . C3 C 0.01230(7) -0.77544(10) -0.28048(6) 0.01331(16) Uani 1 1 d . . . C4 C 0.00093(7) -0.91708(10) -0.29948(6) 0.01490(17) Uani 1 1 d . . . C5 C 0.04873(9) -0.98706(11) -0.36046(7) 0.01829(19) Uani 1 1 d . . . H5 H 0.0988 -0.9481 -0.3948 0.022 Uiso 1 1 calc R . . C6 C 0.02147(10) -1.11591(12) -0.37004(7) 0.0231(2) Uani 1 1 d . . . H6 H 0.0536 -1.1658 -0.4111 0.028 Uiso 1 1 calc R . . C7 C -0.05270(10) -1.17236(12) -0.31970(8) 0.0250(2) Uani 1 1 d . . . H7 H -0.0697 -1.2606 -0.3266 0.030 Uiso 1 1 calc R . . C8 C -0.10206(9) -1.10162(11) -0.25957(7) 0.0214(2) Uani 1 1 d . . . H8 H -0.1534 -1.1396 -0.2260 0.026 Uiso 1 1 calc R . . C9 C -0.07358(8) -0.97354(10) -0.25035(6) 0.01621(18) Uani 1 1 d . . . N10 N -0.15439(7) -0.67522(9) -0.26456(5) 0.01421(15) Uani 1 1 d . . . C11 C -0.13631(8) -0.68114(10) -0.35015(6) 0.01456(17) Uani 1 1 d . . . C12 C -0.01761(8) -0.69742(10) -0.35748(6) 0.01422(17) Uani 1 1 d . . . H12 H 0.0009 -0.7458 -0.4076 0.017 Uiso 1 1 calc R . . C13 C -0.17652(8) -0.56741(11) -0.40001(7) 0.01746(19) Uani 1 1 d . . . N14 N -0.22527(7) -0.46982(9) -0.36094(6) 0.01839(17) Uani 1 1 d . . . C15 C -0.27363(8) -0.49216(10) -0.28290(7) 0.01633(18) Uani 1 1 d . . . H15 H -0.3445 -0.5297 -0.2905 0.020 Uiso 1 1 calc R . . C16 C -0.20891(8) -0.57875(10) -0.22725(7) 0.01632(18) Uani 1 1 d . . . C17 C -0.27459(10) -0.37132(13) -0.41202(8) 0.0244(2) Uani 1 1 d . . . H17A H -0.2307 -0.3544 -0.4592 0.037 Uiso 1 1 calc R . . H17B H -0.2832 -0.2919 -0.3809 0.037 Uiso 1 1 calc R . . H17C H -0.3427 -0.4021 -0.4300 0.037 Uiso 1 1 calc R . . O1 O -0.15895(7) -0.56862(9) -0.47232(5) 0.02372(17) Uani 1 1 d . . . O2 O -0.20776(7) -0.56197(9) -0.15498(5) 0.02371(17) Uani 1 1 d . . . N1' N 0.27569(7) -0.76713(9) -0.18987(6) 0.01522(16) Uani 1 1 d . . . C2' C 0.19613(8) -0.82544(10) -0.23353(6) 0.01557(17) Uani 1 1 d . . . H2' H 0.1980 -0.9108 -0.2540 0.019 Uiso 1 1 calc R . . C3' C 0.11539(8) -0.74243(10) -0.24255(6) 0.01415(17) Uani 1 1 d . . . C4' C 0.14365(8) -0.62453(10) -0.20072(6) 0.01426(17) Uani 1 1 d . . . C5' C 0.09133(8) -0.50849(11) -0.18573(7) 0.01772(19) Uani 1 1 d . . . H5' H 0.0231 -0.4950 -0.2058 0.021 Uiso 1 1 calc R . . C6' C 0.14113(9) -0.41406(12) -0.14107(7) 0.0209(2) Uani 1 1 d . . . H6' H 0.1060 -0.3358 -0.1296 0.025 Uiso 1 1 calc R . . C7' C 0.24256(9) -0.43215(11) -0.11250(7) 0.0201(2) Uani 1 1 d . . . H7' H 0.2755 -0.3648 -0.0834 0.024 Uiso 1 1 calc R . . C8' C 0.29599(8) -0.54600(11) -0.12567(7) 0.01736(18) Uani 1 1 d . . . H8' H 0.3647 -0.5581 -0.1061 0.021 Uiso 1 1 calc R . . C9' C 0.24448(8) -0.64228(10) -0.16901(6) 0.01445(17) Uani 1 1 d . . . O3 O -0.28101(6) -0.37049(8) -0.24383(5) 0.01881(15) Uani 1 1 d . . . O4 O -0.42965(7) -0.43707(9) -0.18418(6) 0.02529(18) Uani 1 1 d . . . C18 C -0.36458(9) -0.35602(11) -0.19340(7) 0.0202(2) Uani 1 1 d . . . C19 C -0.36273(10) -0.22687(13) -0.15384(8) 0.0266(2) Uani 1 1 d . . . H19A H -0.3831 -0.1610 -0.1931 0.040 Uiso 1 1 calc R . . H19B H -0.2925 -0.2087 -0.1341 0.040 Uiso 1 1 calc R . . H19C H -0.4114 -0.2262 -0.1084 0.040 Uiso 1 1 calc R . . O5 O -0.17551(6) -0.80063(8) -0.38268(5) 0.01747(14) Uani 1 1 d . . . O6 O -0.33867(6) -0.72676(9) -0.36943(6) 0.02405(17) Uani 1 1 d . . . C20 C -0.28105(9) -0.81418(12) -0.38442(7) 0.0201(2) Uani 1 1 d . . . C21 C -0.31180(10) -0.94855(14) -0.40513(9) 0.0301(3) Uani 1 1 d . . . H21A H -0.3382 -0.9917 -0.3567 0.045 Uiso 1 1 calc R . . H21B H -0.2513 -0.9953 -0.4257 0.045 Uiso 1 1 calc R . . H21C H -0.3661 -0.9469 -0.4466 0.045 Uiso 1 1 calc R . . O7 O 0.42851(6) -0.76682(8) -0.12437(5) 0.01788(14) Uani 1 1 d . . . O8 O 0.38128(7) -0.94252(9) -0.19770(6) 0.02374(17) Uani 1 1 d . . . C22 C 0.36668(8) -0.83561(11) -0.17177(7) 0.01673(18) Uani 1 1 d . . . C23 C 0.53580(8) -0.81308(11) -0.10599(7) 0.01720(18) Uani 1 1 d . . . C24 C 0.59481(9) -0.83049(14) -0.18468(7) 0.0253(2) Uani 1 1 d . . . H24A H 0.5623 -0.8991 -0.2165 0.038 Uiso 1 1 calc R . . H24B H 0.6670 -0.8536 -0.1728 0.038 Uiso 1 1 calc R . . H24C H 0.5931 -0.7500 -0.2155 0.038 Uiso 1 1 calc R . . C25 C 0.57987(9) -0.70274(12) -0.05686(8) 0.0224(2) Uani 1 1 d . . . H25A H 0.5764 -0.6233 -0.0886 0.034 Uiso 1 1 calc R . . H25B H 0.6524 -0.7212 -0.0430 0.034 Uiso 1 1 calc R . . H25C H 0.5394 -0.6924 -0.0072 0.034 Uiso 1 1 calc R . . C26 C 0.53051(9) -0.93551(12) -0.05599(7) 0.0231(2) Uani 1 1 d . . . H26A H 0.4910 -0.9191 -0.0065 0.035 Uiso 1 1 calc R . . H26B H 0.6010 -0.9632 -0.0419 0.035 Uiso 1 1 calc R . . H26C H 0.4961 -1.0032 -0.0874 0.035 Uiso 1 1 calc R . . S1 S -0.119554(19) -0.91479(2) -0.097407(15) 0.01610(5) Uani 1 1 d . . . O9 O -0.16593(7) -1.03969(9) -0.09105(5) 0.02258(16) Uani 1 1 d . . . O10 O -0.16588(7) -0.80575(9) -0.05904(5) 0.02173(16) Uani 1 1 d . . . C27 C 0.01079(8) -0.92501(11) -0.06705(6) 0.01644(18) Uani 1 1 d . . . C28 C 0.05922(9) -0.81614(12) -0.03571(7) 0.0210(2) Uani 1 1 d . . . H28 H 0.0221 -0.7376 -0.0303 0.025 Uiso 1 1 calc R . . C29 C 0.16276(10) -0.82419(13) -0.01239(7) 0.0250(2) Uani 1 1 d . . . H29 H 0.1970 -0.7509 0.0093 0.030 Uiso 1 1 calc R . . C30 C 0.21617(9) -0.93959(14) -0.02088(8) 0.0263(2) Uani 1 1 d . . . H30 H 0.2866 -0.9451 -0.0042 0.032 Uiso 1 1 calc R . . C31 C 0.16747(10) -1.04708(13) -0.05352(8) 0.0267(2) Uani 1 1 d . . . H31 H 0.2050 -1.1252 -0.0597 0.032 Uiso 1 1 calc R . . C32 C 0.06411(9) -1.04054(11) -0.07715(8) 0.0214(2) Uani 1 1 d . . . H32 H 0.0304 -1.1134 -0.0998 0.026 Uiso 1 1 calc R . . O11 O 0.02661(6) -0.57134(8) -0.35836(5) 0.01605(14) Uani 1 1 d . . . O12 O 0.15758(7) -0.64835(10) -0.43478(7) 0.0299(2) Uani 1 1 d . . . C33 C 0.11673(8) -0.55979(12) -0.40137(7) 0.0201(2) Uani 1 1 d . . . C34 C 0.15435(10) -0.42389(13) -0.40066(9) 0.0288(2) Uani 1 1 d . . . H34A H 0.2295 -0.4225 -0.4096 0.043 Uiso 1 1 calc R . . H34B H 0.1386 -0.3846 -0.3483 0.043 Uiso 1 1 calc R . . H34C H 0.1196 -0.3754 -0.4437 0.043 Uiso 1 1 calc R . . O1S O -0.52660(12) -0.48150(12) -0.43527(8) 0.0468(3) Uani 1 1 d . . . C1S C -0.57166(12) -0.69651(15) -0.46698(9) 0.0328(3) Uani 1 1 d . . . H1S1 H -0.5585 -0.6695 -0.5228 0.049 Uiso 1 1 calc R . . H1S2 H -0.6432 -0.7277 -0.4623 0.049 Uiso 1 1 calc R . . H1S3 H -0.5235 -0.7656 -0.4523 0.049 Uiso 1 1 calc R . . C2S C -0.55617(10) -0.58476(13) -0.41141(8) 0.0255(2) Uani 1 1 d . . . C3S C -0.58143(12) -0.6075(2) -0.32464(9) 0.0411(4) Uani 1 1 d . . . H3S1 H -0.5599 -0.5328 -0.2926 0.062 Uiso 1 1 calc R . . H3S2 H -0.5446 -0.6842 -0.3056 0.062 Uiso 1 1 calc R . . H3S3 H -0.6564 -0.6204 -0.3188 0.062 Uiso 1 1 calc R . . O2S O -0.48184(9) -0.15832(16) -0.32126(7) 0.0459(3) Uani 1 1 d . . . C4S C -0.63804(13) -0.23369(17) -0.26293(11) 0.0392(3) Uani 1 1 d . . . H4S1 H -0.5910 -0.2761 -0.2247 0.059 Uiso 1 1 calc R . . H4S2 H -0.6795 -0.2987 -0.2912 0.059 Uiso 1 1 calc R . . H4S3 H -0.6843 -0.1753 -0.2335 0.059 Uiso 1 1 calc R . . C5S C -0.57583(12) -0.15853(16) -0.32316(9) 0.0332(3) Uani 1 1 d . . . C6S C -0.63456(16) -0.0821(3) -0.38513(12) 0.0574(6) Uani 1 1 d . . . H6S1 H -0.5855 -0.0331 -0.4183 0.086 Uiso 1 1 calc R . . H6S2 H -0.6821 -0.0227 -0.3579 0.086 Uiso 1 1 calc R . . H6S3 H -0.6744 -0.1406 -0.4197 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0149(4) 0.0158(4) 0.0149(4) 0.0005(3) 0.0020(3) -0.0002(3) C2 0.0113(4) 0.0155(4) 0.0150(4) -0.0004(3) 0.0010(3) 0.0007(3) C3 0.0110(4) 0.0148(4) 0.0141(4) -0.0007(3) 0.0007(3) 0.0002(3) C4 0.0132(4) 0.0152(4) 0.0163(4) -0.0019(4) 0.0001(3) -0.0003(3) C5 0.0177(5) 0.0179(5) 0.0192(5) -0.0031(4) 0.0029(4) -0.0002(4) C6 0.0274(6) 0.0190(5) 0.0231(5) -0.0059(4) 0.0042(4) 0.0001(4) C7 0.0302(6) 0.0177(5) 0.0271(6) -0.0050(4) 0.0043(4) -0.0052(4) C8 0.0224(5) 0.0181(5) 0.0235(5) -0.0014(4) 0.0027(4) -0.0049(4) C9 0.0155(4) 0.0165(4) 0.0166(4) -0.0014(4) 0.0000(3) -0.0006(3) N10 0.0125(3) 0.0175(4) 0.0126(3) 0.0004(3) 0.0012(3) 0.0026(3) C11 0.0122(4) 0.0180(4) 0.0135(4) -0.0013(3) -0.0002(3) -0.0001(3) C12 0.0119(4) 0.0159(4) 0.0148(4) -0.0001(3) 0.0011(3) 0.0001(3) C13 0.0130(4) 0.0216(5) 0.0178(4) 0.0029(4) -0.0008(3) 0.0006(4) N14 0.0173(4) 0.0197(4) 0.0182(4) 0.0042(3) 0.0007(3) 0.0033(3) C15 0.0152(4) 0.0153(4) 0.0186(4) 0.0006(4) 0.0011(3) 0.0023(3) C16 0.0142(4) 0.0159(4) 0.0189(4) -0.0001(4) 0.0017(3) 0.0022(3) C17 0.0250(5) 0.0240(5) 0.0243(5) 0.0072(4) -0.0029(4) 0.0053(4) O1 0.0230(4) 0.0324(5) 0.0158(3) 0.0035(3) 0.0003(3) 0.0039(3) O2 0.0279(4) 0.0260(4) 0.0172(4) -0.0022(3) 0.0003(3) 0.0093(3) N1' 0.0113(3) 0.0146(4) 0.0197(4) -0.0012(3) -0.0017(3) 0.0015(3) C2' 0.0128(4) 0.0145(4) 0.0194(4) -0.0013(3) 0.0001(3) -0.0004(3) C3' 0.0124(4) 0.0148(4) 0.0152(4) -0.0013(3) 0.0010(3) -0.0002(3) C4' 0.0126(4) 0.0148(4) 0.0154(4) -0.0008(3) 0.0008(3) 0.0007(3) C5' 0.0150(4) 0.0176(5) 0.0206(5) -0.0026(4) -0.0012(4) 0.0035(4) C6' 0.0201(5) 0.0180(5) 0.0245(5) -0.0054(4) -0.0013(4) 0.0042(4) C7' 0.0203(5) 0.0185(5) 0.0214(5) -0.0056(4) -0.0021(4) 0.0008(4) C8' 0.0156(4) 0.0174(4) 0.0191(4) -0.0026(4) -0.0023(3) 0.0000(3) C9' 0.0129(4) 0.0148(4) 0.0156(4) -0.0004(3) 0.0007(3) 0.0007(3) O3 0.0157(3) 0.0157(3) 0.0250(4) -0.0012(3) 0.0022(3) 0.0013(3) O4 0.0212(4) 0.0235(4) 0.0312(4) -0.0024(3) 0.0064(3) -0.0010(3) C18 0.0177(5) 0.0202(5) 0.0228(5) -0.0005(4) 0.0017(4) 0.0041(4) C19 0.0260(5) 0.0225(5) 0.0314(6) -0.0069(5) 0.0025(5) 0.0013(4) O5 0.0137(3) 0.0211(4) 0.0175(3) -0.0039(3) -0.0006(3) -0.0017(3) O6 0.0152(3) 0.0308(4) 0.0262(4) -0.0037(3) -0.0009(3) -0.0004(3) C20 0.0160(4) 0.0279(5) 0.0164(4) -0.0021(4) -0.0005(3) -0.0044(4) C21 0.0243(6) 0.0305(6) 0.0355(7) -0.0116(5) 0.0013(5) -0.0084(5) O7 0.0120(3) 0.0179(3) 0.0237(4) -0.0011(3) -0.0025(3) 0.0019(3) O8 0.0189(4) 0.0203(4) 0.0321(4) -0.0062(3) -0.0048(3) 0.0057(3) C22 0.0116(4) 0.0183(5) 0.0203(5) 0.0012(4) -0.0006(3) 0.0015(3) C23 0.0103(4) 0.0199(5) 0.0214(5) 0.0018(4) -0.0017(3) 0.0031(3) C24 0.0147(4) 0.0392(7) 0.0221(5) 0.0001(5) 0.0021(4) 0.0031(4) C25 0.0159(4) 0.0225(5) 0.0287(6) -0.0011(4) -0.0038(4) -0.0005(4) C26 0.0239(5) 0.0203(5) 0.0250(5) 0.0038(4) -0.0033(4) 0.0029(4) S1 0.01461(10) 0.01829(11) 0.01540(10) 0.00165(9) 0.00263(8) 0.00079(9) O9 0.0223(4) 0.0229(4) 0.0226(4) 0.0042(3) 0.0027(3) -0.0060(3) O10 0.0213(4) 0.0262(4) 0.0177(4) 0.0005(3) 0.0058(3) 0.0073(3) C27 0.0172(4) 0.0175(5) 0.0145(4) 0.0022(4) 0.0003(3) 0.0013(4) C28 0.0248(5) 0.0202(5) 0.0179(5) -0.0007(4) -0.0001(4) 0.0000(4) C29 0.0264(6) 0.0288(6) 0.0198(5) 0.0004(4) -0.0040(4) -0.0054(5) C30 0.0190(5) 0.0351(7) 0.0250(5) 0.0090(5) -0.0041(4) -0.0008(4) C31 0.0228(5) 0.0254(6) 0.0318(6) 0.0081(5) -0.0008(4) 0.0063(4) C32 0.0221(5) 0.0159(5) 0.0263(5) 0.0033(4) 0.0004(4) 0.0021(4) O11 0.0142(3) 0.0160(3) 0.0180(3) 0.0003(3) 0.0014(3) -0.0002(3) O12 0.0232(4) 0.0264(4) 0.0401(5) -0.0048(4) 0.0141(4) -0.0022(3) C33 0.0162(5) 0.0216(5) 0.0225(5) 0.0030(4) 0.0030(4) -0.0015(4) C34 0.0274(6) 0.0199(5) 0.0390(7) 0.0010(5) 0.0079(5) -0.0060(5) O1S 0.0583(8) 0.0345(6) 0.0476(7) 0.0047(5) -0.0040(6) -0.0161(5) C1S 0.0302(6) 0.0325(7) 0.0356(7) -0.0066(5) -0.0051(5) -0.0015(5) C2S 0.0211(5) 0.0312(6) 0.0242(5) 0.0003(5) -0.0030(4) -0.0017(4) C3S 0.0302(7) 0.0701(12) 0.0231(6) 0.0003(7) 0.0004(5) -0.0006(7) O2S 0.0289(5) 0.0721(9) 0.0366(6) 0.0103(6) 0.0005(4) -0.0031(5) C4S 0.0340(7) 0.0342(7) 0.0495(9) -0.0018(6) 0.0033(6) -0.0095(6) C5S 0.0302(6) 0.0408(8) 0.0287(6) -0.0040(6) -0.0005(5) -0.0025(6) C6S 0.0415(9) 0.0948(17) 0.0358(8) 0.0102(10) 0.0011(7) 0.0172(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C9 1.4384(13) . ? N1 C2 1.4858(13) . ? N1 S1 1.6755(9) . ? C2 N10 1.4614(13) . ? C2 C3 1.5699(14) . ? C3 C3' 1.5077(14) . ? C3 C4 1.5126(15) . ? C3 C12 1.5583(14) . ? C4 C5 1.3885(14) . ? C4 C9 1.3886(14) . ? C5 C6 1.3937(16) . ? C6 C7 1.3974(17) . ? C7 C8 1.3915(17) . ? C8 C9 1.3894(15) . ? N10 C16 1.3715(13) . ? N10 C11 1.4370(13) . ? C11 O5 1.4446(13) . ? C11 C13 1.5316(15) . ? C11 C12 1.5431(14) . ? C12 O11 1.4291(12) . ? C13 O1 1.2180(14) . ? C13 N14 1.3574(14) . ? N14 C15 1.4530(14) . ? N14 C17 1.4714(15) . ? C15 O3 1.4236(13) . ? C15 C16 1.5335(15) . ? C16 O2 1.2086(14) . ? N1' C2' 1.3921(13) . ? N1' C9' 1.4020(13) . ? N1' C22 1.4033(13) . ? C2' C3' 1.3595(14) . ? C3' C4' 1.4537(14) . ? C4' C5' 1.4039(14) . ? C4' C9' 1.4124(14) . ? C5' C6' 1.3857(15) . ? C6' C7' 1.4015(15) . ? C7' C8' 1.3863(15) . ? C8' C9' 1.3983(14) . ? O3 C18 1.3710(13) . ? O4 C18 1.1983(15) . ? C18 C19 1.4939(17) . ? O5 C20 1.3669(13) . ? O6 C20 1.1994(15) . ? C20 C21 1.4917(18) . ? O7 C22 1.3264(13) . ? O7 C23 1.4942(12) . ? O8 C22 1.2062(14) . ? C23 C25 1.5159(16) . ? C23 C24 1.5193(16) . ? C23 C26 1.5196(16) . ? S1 O10 1.4300(9) . ? S1 O9 1.4331(9) . ? S1 C27 1.7551(11) . ? C27 C28 1.3922(16) . ? C27 C32 1.3937(15) . ? C28 C29 1.3905(17) . ? C29 C30 1.3900(19) . ? C30 C31 1.390(2) . ? C31 C32 1.3888(17) . ? O11 C33 1.3676(13) . ? O12 C33 1.1962(15) . ? C33 C34 1.4936(17) . ? O1S C2S 1.2056(18) . ? C1S C2S 1.4948(19) . ? C2S C3S 1.4915(19) . ? O2S C5S 1.2110(19) . ? C4S C5S 1.499(2) . ? C5S C6S 1.501(2) . ? 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 C9 N1 C2 108.25(8) . . ? C9 N1 S1 117.91(7) . . ? C2 N1 S1 116.55(7) . . ? N10 C2 N1 112.99(8) . . ? N10 C2 C3 104.71(8) . . ? N1 C2 C3 105.98(8) . . ? C3' C3 C4 113.15(8) . . ? C3' C3 C12 116.02(8) . . ? C4 C3 C12 108.23(8) . . ? C3' C3 C2 110.60(8) . . ? C4 C3 C2 102.64(8) . . ? C12 C3 C2 105.07(8) . . ? C5 C4 C9 120.75(10) . . ? C5 C4 C3 128.18(9) . . ? C9 C4 C3 110.89(9) . . ? C4 C5 C6 118.31(10) . . ? C5 C6 C7 120.54(11) . . ? C8 C7 C6 121.17(11) . . ? C9 C8 C7 117.65(11) . . ? C4 C9 C8 121.56(10) . . ? C4 C9 N1 110.84(9) . . ? C8 C9 N1 127.46(10) . . ? C16 N10 C11 123.96(9) . . ? C16 N10 C2 120.38(9) . . ? C11 N10 C2 111.95(8) . . ? N10 C11 O5 110.31(8) . . ? N10 C11 C13 116.29(9) . . ? O5 C11 C13 110.19(8) . . ? N10 C11 C12 104.11(8) . . ? O5 C11 C12 102.85(8) . . ? C13 C11 C12 112.14(8) . . ? O11 C12 C11 107.16(8) . . ? O11 C12 C3 112.80(8) . . ? C11 C12 C3 103.70(8) . . ? O1 C13 N14 124.21(11) . . ? O1 C13 C11 117.27(10) . . ? N14 C13 C11 118.47(9) . . ? C13 N14 C15 120.19(9) . . ? C13 N14 C17 116.49(10) . . ? C15 N14 C17 115.88(9) . . ? O3 C15 N14 106.89(9) . . ? O3 C15 C16 106.58(9) . . ? N14 C15 C16 113.22(9) . . ? O2 C16 N10 123.04(10) . . ? O2 C16 C15 121.03(10) . . ? N10 C16 C15 115.92(9) . . ? C2' N1' C9' 108.65(8) . . ? C2' N1' C22 120.27(9) . . ? C9' N1' C22 131.04(9) . . ? C3' C2' N1' 110.07(9) . . ? C2' C3' C4' 106.96(9) . . ? C2' C3' C3 125.07(9) . . ? C4' C3' C3 127.60(9) . . ? C5' C4' C9' 119.21(9) . . ? C5' C4' C3' 133.52(9) . . ? C9' C4' C3' 107.24(9) . . ? C6' C5' C4' 118.75(10) . . ? C5' C6' C7' 121.03(10) . . ? C8' C7' C6' 121.62(10) . . ? C7' C8' C9' 117.15(10) . . ? C8' C9' N1' 130.76(9) . . ? C8' C9' C4' 122.18(9) . . ? N1' C9' C4' 107.05(9) . . ? C18 O3 C15 115.26(9) . . ? O4 C18 O3 123.37(11) . . ? O4 C18 C19 125.94(11) . . ? O3 C18 C19 110.69(10) . . ? C20 O5 C11 116.34(8) . . ? O6 C20 O5 122.21(11) . . ? O6 C20 C21 126.36(11) . . ? O5 C20 C21 111.42(10) . . ? C22 O7 C23 120.09(9) . . ? O8 C22 O7 127.84(10) . . ? O8 C22 N1' 121.46(10) . . ? O7 C22 N1' 110.70(9) . . ? O7 C23 C25 102.20(8) . . ? O7 C23 C24 109.10(9) . . ? C25 C23 C24 111.25(10) . . ? O7 C23 C26 109.78(9) . . ? C25 C23 C26 111.02(9) . . ? C24 C23 C26 112.94(10) . . ? O10 S1 O9 120.75(5) . . ? O10 S1 N1 105.62(5) . . ? O9 S1 N1 105.68(5) . . ? O10 S1 C27 108.69(5) . . ? O9 S1 C27 108.84(5) . . ? N1 S1 C27 106.32(5) . . ? C28 C27 C32 121.64(10) . . ? C28 C27 S1 119.04(9) . . ? C32 C27 S1 119.29(9) . . ? C29 C28 C27 118.92(11) . . ? C30 C29 C28 119.91(12) . . ? C29 C30 C31 120.64(11) . . ? C32 C31 C30 120.13(12) . . ? C31 C32 C27 118.74(11) . . ? C33 O11 C12 115.11(8) . . ? O12 C33 O11 123.16(11) . . ? O12 C33 C34 126.08(10) . . ? O11 C33 C34 110.76(10) . . ? O1S C2S C3S 121.72(14) . . ? O1S C2S C1S 122.17(13) . . ? C3S C2S C1S 116.09(13) . . ? O2S C5S C4S 121.25(15) . . ? O2S C5S C6S 121.31(16) . . ? C4S C5S C6S 117.44(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.382 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.044 _database_code_depnum_ccdc_archive 'CCDC 933937' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_x8_13026 #TrackingRef 'X8_13026-nitrobenzoylatedbionectinA.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H21 N5 O6 S2' _chemical_formula_weight 599.63 _chemical_absolute_configuration ad 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.6928(7) _cell_length_b 11.2669(6) _cell_length_c 20.6483(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.6760(10) _cell_angle_gamma 90.00 _cell_volume 2701.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9982 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 31.52 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.252 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9560 _exptl_absorpt_correction_T_max 0.9728 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. Please acknowledge this grant in all publications of this structure. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 97606 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 31.00 _reflns_number_total 17143 _reflns_number_gt 15920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 17143 _refine_ls_number_parameters 1207 _refine_ls_number_restraints 3313 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 1.231 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.002 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 -0.74395(11) -0.49430(8) -0.42072(5) 0.0182(2) Uani 0.812(5) 1 d PU A 1 S2 S -0.70411(7) -0.63513(10) -0.47867(6) 0.0212(2) Uani 0.812(5) 1 d PU A 1 N1 N -0.6408(2) -0.4014(2) -0.62912(15) 0.0160(4) Uani 0.812(5) 1 d PDU A 1 H1 H -0.6344 -0.3251 -0.6370 0.019 Uiso 0.812(5) 1 calc PR A 1 C2 C -0.7465(4) -0.4684(4) -0.6343(4) 0.0132(8) Uani 0.812(5) 1 d PDU A 1 H2 H -0.8034 -0.4360 -0.6698 0.016 Uiso 0.812(5) 1 calc PR A 1 C3 C -0.7110(2) -0.5971(2) -0.65040(15) 0.0111(4) Uani 0.812(5) 1 d PDU A 1 C4 C -0.5854(2) -0.5962(2) -0.62042(15) 0.0142(5) Uani 0.812(5) 1 d PDU A 1 C5 C -0.5090(2) -0.6889(2) -0.60583(14) 0.0173(5) Uani 0.812(5) 1 d PDU A 1 H5 H -0.5331 -0.7687 -0.6134 0.021 Uiso 0.812(5) 1 calc PR A 1 C6 C -0.3949(3) -0.6632(4) -0.5796(2) 0.0245(8) Uani 0.812(5) 1 d PDU A 1 H6 H -0.3416 -0.7255 -0.5683 0.029 Uiso 0.812(5) 1 calc PR A 1 C7 C -0.3614(3) -0.5457(4) -0.57048(18) 0.0268(7) Uani 0.812(5) 1 d PDU A 1 H7 H -0.2837 -0.5286 -0.5543 0.032 Uiso 0.812(5) 1 calc PR A 1 C8 C -0.4379(3) -0.4521(3) -0.58434(19) 0.0220(7) Uani 0.812(5) 1 d PDU A 1 H8 H -0.4141 -0.3721 -0.5770 0.026 Uiso 0.812(5) 1 calc PR A 1 C9 C -0.5502(3) -0.4794(3) -0.60926(18) 0.0150(6) Uani 0.812(5) 1 d PDU A 1 C12 C -0.7848(2) -0.6788(3) -0.60955(17) 0.0138(5) Uani 0.812(5) 1 d PU A 1 H12 H -0.7439 -0.7541 -0.5956 0.017 Uiso 0.812(5) 1 calc PR A 1 N10 N -0.7996(3) -0.4815(3) -0.57270(15) 0.0121(4) Uani 0.812(5) 1 d PDU A 1 C11 C -0.8111(3) -0.6024(3) -0.55068(14) 0.0133(5) Uani 0.812(5) 1 d PDU A 1 C13 C -0.9257(3) -0.6228(3) -0.52316(12) 0.0184(5) Uani 0.812(5) 1 d PDU A 1 N14 N -0.9562(3) -0.5283(4) -0.4886(2) 0.0149(6) Uani 0.812(5) 1 d PDU A 1 C15 C -0.8714(5) -0.4370(5) -0.4730(2) 0.0129(7) Uani 0.812(5) 1 d PDU A 1 H15 H -0.9064 -0.3703 -0.4502 0.016 Uiso 0.812(5) 1 calc PR A 1 C16 C -0.8260(4) -0.3904(2) -0.5343(2) 0.0124(5) Uani 0.812(5) 1 d PDU A 1 C17 C -1.0554(4) -0.5319(5) -0.4513(3) 0.0206(9) Uani 0.812(5) 1 d PDU A 1 H17A H -1.1077 -0.5956 -0.4682 0.031 Uiso 0.812(5) 1 calc PR A 1 H17B H -1.0961 -0.4557 -0.4556 0.031 Uiso 0.812(5) 1 calc PR A 1 H17C H -1.0289 -0.5467 -0.4053 0.031 Uiso 0.812(5) 1 calc PR A 1 O18 O -0.9784(3) -0.7165(3) -0.52990(13) 0.0321(6) Uani 0.812(5) 1 d PDU A 1 O19 O -0.8088(3) -0.2855(2) -0.5451(2) 0.0156(5) Uani 0.812(5) 1 d PDU A 1 O20 O -0.8952(4) -0.7004(5) -0.6463(2) 0.0148(6) Uani 0.812(5) 1 d PU A 1 C21 C -0.9094(3) -0.8091(3) -0.67467(19) 0.0142(6) Uani 0.812(5) 1 d PU A 1 O22 O -0.83418(19) -0.8830(3) -0.67333(17) 0.0263(5) Uani 0.812(5) 1 d PU A 1 C23 C -1.0279(3) -0.8256(4) -0.7079(2) 0.0163(7) Uani 0.812(5) 1 d PDU A 1 C24 C -1.1206(2) -0.7584(3) -0.69166(15) 0.0184(5) Uani 0.812(5) 1 d PDU A 1 H24 H -1.1091 -0.7007 -0.6580 0.022 Uiso 0.812(5) 1 calc PR A 1 C25 C -1.2301(2) -0.7758(3) -0.72476(15) 0.0216(5) Uani 0.812(5) 1 d PDU A 1 H25 H -1.2944 -0.7320 -0.7135 0.026 Uiso 0.812(5) 1 calc PR A 1 C26 C -1.2424(2) -0.8591(4) -0.77463(18) 0.0186(7) Uani 0.812(5) 1 d PDU A 1 C27 C -1.1518(4) -0.9299(5) -0.7903(3) 0.0254(8) Uani 0.812(5) 1 d PDU A 1 H27 H -1.1635 -0.9885 -0.8235 0.030 Uiso 0.812(5) 1 calc PR A 1 C28 C -1.0444(3) -0.9122(5) -0.7561(3) 0.0241(7) Uani 0.812(5) 1 d PDU A 1 H28 H -0.9813 -0.9597 -0.7656 0.029 Uiso 0.812(5) 1 calc PR A 1 N29 N -1.3566(3) -0.8745(3) -0.81194(14) 0.0239(5) Uani 0.812(5) 1 d PU A 1 O30 O -1.3768(3) -0.9602(3) -0.84898(16) 0.0381(6) Uani 0.812(5) 1 d PU A 1 O31 O -1.4317(2) -0.8010(3) -0.80417(14) 0.0325(5) Uani 0.812(5) 1 d PU A 1 N1' N -0.6849(5) -0.6933(7) -0.8191(3) 0.0210(3) Uani 0.812(5) 1 d PDU A 1 H2N H -0.651(3) -0.729(3) -0.8508(17) 0.025 Uiso 0.812(5) 1 d P A 1 C2' C -0.6434(4) -0.6775(4) -0.7548(3) 0.0161(7) Uani 0.812(5) 1 d PDU A 1 H2' H -0.5686 -0.6999 -0.7358 0.019 Uiso 0.812(5) 1 calc PR A 1 C3' C -0.7252(4) -0.6247(4) -0.7220(2) 0.0147(7) Uani 0.812(5) 1 d PDU A 1 C4' C -0.8256(6) -0.6070(10) -0.7692(3) 0.0181(6) Uani 0.812(5) 1 d PDU A 1 C5' C -0.9370(3) -0.5610(3) -0.76711(18) 0.0201(8) Uani 0.812(5) 1 d PDU A 1 H5' H -0.9594 -0.5313 -0.7274 0.024 Uiso 0.812(5) 1 calc PR A 1 C6' C -1.0136(2) -0.5594(3) -0.82355(13) 0.0237(6) Uani 0.812(5) 1 d PDU A 1 H6' H -1.0890 -0.5287 -0.8223 0.028 Uiso 0.812(5) 1 calc PR A 1 C7' C -0.9811(2) -0.6027(3) -0.88286(13) 0.0269(6) Uani 0.812(5) 1 d PDU A 1 H7' H -1.0346 -0.5992 -0.9211 0.032 Uiso 0.812(5) 1 calc PR A 1 C8' C -0.8729(3) -0.6504(3) -0.88647(16) 0.0249(7) Uani 0.812(5) 1 d PDU A 1 H8' H -0.8515 -0.6803 -0.9263 0.030 Uiso 0.812(5) 1 calc PR A 1 C9' C -0.7962(3) -0.6527(4) -0.8290(2) 0.0192(8) Uani 0.812(5) 1 d PDU A 1 S1B S -0.7687(7) -0.5010(9) -0.4185(4) 0.063(3) Uani 0.188(5) 1 d PU A 2 S2B S -0.7234(11) -0.6609(8) -0.4864(4) 0.073(3) Uani 0.188(5) 1 d PU A 2 N1B N -0.6351(12) -0.4281(11) -0.6211(8) 0.0160(4) Uani 0.188(5) 1 d PDU A 2 H1B H -0.6222 -0.3512 -0.6214 0.019 Uiso 0.188(5) 1 calc PR A 2 C2B C -0.7450(14) -0.4843(16) -0.6389(17) 0.013(3) Uani 0.188(5) 1 d PDU A 2 H2B H -0.7907 -0.4480 -0.6778 0.016 Uiso 0.188(5) 1 calc PR A 2 C3B C -0.7257(12) -0.6186(13) -0.6454(8) 0.0111(4) Uani 0.188(5) 1 d PDU A 2 C4B C -0.5986(11) -0.6219(12) -0.6184(8) 0.0148(8) Uani 0.188(5) 1 d PDU A 2 C5B C -0.5281(11) -0.7175(12) -0.6052(7) 0.0173(5) Uani 0.188(5) 1 d PDU A 2 H5B H -0.5552 -0.7958 -0.6147 0.021 Uiso 0.188(5) 1 calc PR A 2 C6B C -0.4145(14) -0.6972(17) -0.5772(10) 0.031(4) Uani 0.188(5) 1 d PDU A 2 H6B H -0.3652 -0.7634 -0.5674 0.037 Uiso 0.188(5) 1 calc PR A 2 C7B C -0.3726(13) -0.5868(16) -0.5635(9) 0.031(3) Uani 0.188(5) 1 d PDU A 2 H7B H -0.2944 -0.5779 -0.5458 0.038 Uiso 0.188(5) 1 calc PR A 2 C8B C -0.4407(13) -0.4866(15) -0.5746(10) 0.029(3) Uani 0.188(5) 1 d PDU A 2 H8B H -0.4147 -0.4084 -0.5640 0.035 Uiso 0.188(5) 1 calc PR A 2 C9B C -0.5537(11) -0.5139(13) -0.6037(10) 0.022(3) Uani 0.188(5) 1 d PDU A 2 C12B C -0.8105(13) -0.6850(18) -0.6161(9) 0.0138(5) Uani 0.188(5) 1 d PU A 2 H12B H -0.7747 -0.7624 -0.6011 0.017 Uiso 0.188(5) 1 calc PR A 2 N10B N -0.8109(18) -0.4973(13) -0.5811(8) 0.0121(4) Uani 0.188(5) 1 d PDU A 2 C11B C -0.8256(15) -0.6208(14) -0.5624(9) 0.029(2) Uani 0.188(5) 1 d PDU A 2 C13B C -0.9423(13) -0.6285(15) -0.5374(7) 0.0184(5) Uani 0.188(5) 1 d PDU A 2 N14B N -0.967(2) -0.540(2) -0.4982(13) 0.027(4) Uani 0.188(5) 1 d PDU A 2 C15B C -0.884(3) -0.448(2) -0.4814(11) 0.019(3) Uani 0.188(5) 1 d PDU A 2 H15B H -0.9224 -0.3774 -0.4647 0.023 Uiso 0.188(5) 1 calc PR A 2 C16B C -0.818(2) -0.4112(13) -0.5393(11) 0.0124(5) Uani 0.188(5) 1 d PDU A 2 C17B C -1.063(3) -0.556(3) -0.4595(17) 0.035(6) Uani 0.188(5) 1 d PDU A 2 H17D H -1.0690 -0.6395 -0.4479 0.052 Uiso 0.188(5) 1 calc PR A 2 H17E H -1.1347 -0.5300 -0.4849 0.052 Uiso 0.188(5) 1 calc PR A 2 H17F H -1.0493 -0.5078 -0.4197 0.052 Uiso 0.188(5) 1 calc PR A 2 O18B O -1.0016(14) -0.7163(14) -0.5467(7) 0.0321(6) Uani 0.188(5) 1 d PDU A 2 O19B O -0.7975(18) -0.3058(12) -0.5482(10) 0.0156(5) Uani 0.188(5) 1 d PDU A 2 O20B O -0.912(2) -0.710(3) -0.6562(13) 0.026(3) Uani 0.188(5) 1 d PU A 2 C21B C -0.9401(17) -0.8181(18) -0.6851(11) 0.025(3) Uani 0.188(5) 1 d PU A 2 O22B O -0.8637(11) -0.8919(16) -0.6715(9) 0.0263(5) Uani 0.188(5) 1 d PU A 2 C23B C -1.0454(16) -0.8200(18) -0.7216(10) 0.026(3) Uani 0.188(5) 1 d PDU A 2 C24B C -1.1315(13) -0.7380(15) -0.7121(8) 0.037(4) Uani 0.188(5) 1 d PDU A 2 H24B H -1.1167 -0.6720 -0.6838 0.044 Uiso 0.188(5) 1 calc PR A 2 C25B C -1.2378(11) -0.7567(12) -0.7453(6) 0.0216(5) Uani 0.188(5) 1 d PDU A 2 H25B H -1.2979 -0.7033 -0.7382 0.026 Uiso 0.188(5) 1 calc PR A 2 C26B C -1.2632(16) -0.8492(16) -0.7889(9) 0.029(3) Uani 0.188(5) 1 d PDU A 2 C27B C -1.1754(18) -0.928(3) -0.7981(16) 0.034(4) Uani 0.188(5) 1 d PDU A 2 H27B H -1.1887 -0.9899 -0.8294 0.041 Uiso 0.188(5) 1 calc PR A 2 C28B C -1.0703(17) -0.917(2) -0.7626(14) 0.033(4) Uani 0.188(5) 1 d PDU A 2 H28B H -1.0134 -0.9765 -0.7659 0.040 Uiso 0.188(5) 1 calc PR A 2 N29B N -1.3725(14) -0.8544(15) -0.8259(8) 0.0239(5) Uani 0.188(5) 1 d PU A 2 O30B O -1.3559(14) -0.9377(16) -0.8618(8) 0.0381(6) Uani 0.188(5) 1 d PU A 2 O31B O -1.4440(11) -0.7850(14) -0.8248(6) 0.0325(5) Uani 0.188(5) 1 d PU A 2 N1'B N -0.685(2) -0.696(3) -0.8185(13) 0.0210(3) Uani 0.188(5) 1 d PDU A 2 H1'B H -0.6477 -0.7314 -0.8478 0.025 Uiso 0.188(5) 1 calc PR A 2 C2'B C -0.651(2) -0.696(2) -0.7524(13) 0.0161(7) Uani 0.188(5) 1 d PDU A 2 H2'B H -0.5821 -0.7297 -0.7317 0.019 Uiso 0.188(5) 1 calc PR A 2 C3'B C -0.733(2) -0.640(2) -0.7211(11) 0.0147(7) Uani 0.188(5) 1 d PDU A 2 C4'B C -0.822(3) -0.602(5) -0.7708(11) 0.0181(6) Uani 0.188(5) 1 d PDU A 2 C5'B C -0.9257(17) -0.539(2) -0.7708(9) 0.0201(8) Uani 0.188(5) 1 d PDU A 2 H5'B H -0.9476 -0.5074 -0.7314 0.024 Uiso 0.188(5) 1 calc PR A 2 C6'B C -0.9938(12) -0.5248(13) -0.8280(6) 0.0237(6) Uani 0.188(5) 1 d PDU A 2 H6'B H -1.0663 -0.4870 -0.8273 0.028 Uiso 0.188(5) 1 calc PR A 2 C7'B C -0.9629(11) -0.5625(14) -0.8877(6) 0.0269(6) Uani 0.188(5) 1 d PDU A 2 H7'B H -1.0131 -0.5492 -0.9265 0.032 Uiso 0.188(5) 1 calc PR A 2 C8'B C -0.8586(13) -0.6195(15) -0.8903(8) 0.0249(7) Uani 0.188(5) 1 d PDU A 2 H8'B H -0.8370 -0.6480 -0.9304 0.030 Uiso 0.188(5) 1 calc PR A 2 C9'B C -0.7859(18) -0.634(2) -0.8318(9) 0.0192(8) Uani 0.188(5) 1 d PDU A 2 S1A S -0.69881(9) -0.03730(8) -0.06794(3) 0.03122(17) Uani 0.877(3) 1 d PU B 1 S2A S -0.72797(10) -0.18427(7) -0.01063(3) 0.02691(17) Uani 0.877(3) 1 d PU B 1 N1A N -0.8768(2) 0.0321(3) 0.10609(15) 0.0269(5) Uani 0.877(3) 1 d PDU B 1 H1A H -0.8991 0.1059 0.0986 0.032 Uiso 0.877(3) 1 calc PR B 1 C2A C -0.7620(2) -0.0029(2) 0.13177(14) 0.0155(4) Uani 0.877(3) 1 d PDU B 1 H2A H -0.7316 0.0485 0.1694 0.019 Uiso 0.877(3) 1 calc PR B 1 C3A C -0.7733(2) -0.13489(19) 0.15377(13) 0.0150(4) Uani 0.877(3) 1 d PDU B 1 C4A C -0.89131(19) -0.1675(3) 0.12061(11) 0.0202(5) Uani 0.877(3) 1 d PDU B 1 C5A C -0.9432(2) -0.2773(3) 0.11478(12) 0.0273(5) Uani 0.877(3) 1 d PDU B 1 H5A H -0.9030 -0.3466 0.1308 0.033 Uiso 0.877(3) 1 calc PR B 1 C6A C -1.0570(2) -0.2843(3) 0.08447(13) 0.0366(6) Uani 0.877(3) 1 d PDU B 1 H6A H -1.0950 -0.3589 0.0800 0.044 Uiso 0.877(3) 1 calc PR B 1 C7A C -1.1138(2) -0.1822(4) 0.06111(13) 0.0372(6) Uani 0.877(3) 1 d PDU B 1 H7A H -1.1915 -0.1876 0.0418 0.045 Uiso 0.877(3) 1 calc PR B 1 C8A C -1.0604(2) -0.0728(3) 0.06513(13) 0.0328(6) Uani 0.877(3) 1 d PDU B 1 H8A H -1.0998 -0.0039 0.0481 0.039 Uiso 0.877(3) 1 calc PR B 1 C9A C -0.9469(2) -0.0659(3) 0.09492(12) 0.0228(5) Uani 0.877(3) 1 d PDU B 1 C12A C -0.6768(2) -0.2065(2) 0.12379(15) 0.0154(5) Uani 0.877(3) 1 d PU B 1 H12A H -0.7054 -0.2862 0.1080 0.018 Uiso 0.877(3) 1 calc PR B 1 N10A N -0.6781(3) -0.0116(3) 0.08319(14) 0.0187(6) Uani 0.877(3) 1 d PDU B 1 C11A C -0.6456(2) -0.1292(2) 0.06735(10) 0.0162(4) Uani 0.877(3) 1 d PDU B 1 C13A C -0.5202(2) -0.1350(2) 0.05146(11) 0.0204(4) Uani 0.877(3) 1 d PDU B 1 N14A N -0.49518(19) -0.0442(2) 0.01271(10) 0.0220(4) Uani 0.877(3) 1 d PDU B 1 C15A C -0.5856(3) 0.0368(2) -0.00938(13) 0.0224(5) Uani 0.877(3) 1 d PDU B 1 H15A H -0.5530 0.1063 -0.0311 0.027 Uiso 0.877(3) 1 calc PR B 1 C16A C -0.6506(3) 0.0797(3) 0.04570(13) 0.0233(6) Uani 0.877(3) 1 d PDU B 1 C17A C -0.3861(3) -0.0397(3) -0.01521(16) 0.0344(6) Uani 0.877(3) 1 d PDU B 1 H17J H -0.3322 0.0121 0.0115 0.052 Uiso 0.877(3) 1 calc PR B 1 H17K H -0.3993 -0.0083 -0.0597 0.052 Uiso 0.877(3) 1 calc PR B 1 H17L H -0.3537 -0.1197 -0.0161 0.052 Uiso 0.877(3) 1 calc PR B 1 O18A O -0.45417(19) -0.21531(18) 0.06877(10) 0.0248(4) Uani 0.877(3) 1 d PDU B 1 O19A O -0.6760(4) 0.1831(3) 0.05477(16) 0.0320(7) Uani 0.877(3) 1 d PDU B 1 O20A O -0.57726(18) -0.21705(18) 0.17178(7) 0.0161(3) Uani 0.877(3) 1 d PDU B 1 C21A C -0.53501(18) -0.3278(2) 0.18136(10) 0.0208(4) Uani 0.877(3) 1 d PDU B 1 O22A O -0.5821(2) -0.41577(17) 0.15801(11) 0.0383(6) Uani 0.877(3) 1 d PDU B 1 C23A C -0.4233(2) -0.3297(3) 0.22498(16) 0.0196(4) Uani 0.877(3) 1 d PDU B 1 C24A C -0.3640(2) -0.2259(2) 0.24310(17) 0.0365(6) Uani 0.877(3) 1 d PDU B 1 H24A H -0.3943 -0.1510 0.2285 0.044 Uiso 0.877(3) 1 calc PR B 1 C25A C -0.2595(2) -0.2327(3) 0.2830(2) 0.0401(7) Uani 0.877(3) 1 d PDU B 1 H25A H -0.2177 -0.1630 0.2964 0.048 Uiso 0.877(3) 1 calc PR B 1 C26A C -0.2186(3) -0.3425(2) 0.30232(11) 0.0224(5) Uani 0.877(3) 1 d PDU B 1 C27A C -0.2757(3) -0.4460(3) 0.28495(18) 0.0382(7) Uani 0.877(3) 1 d PDU B 1 H27A H -0.2452 -0.5204 0.3002 0.046 Uiso 0.877(3) 1 calc PR B 1 C28A C -0.3795(3) -0.4396(3) 0.24439(18) 0.0361(7) Uani 0.877(3) 1 d PDU B 1 H28A H -0.4197 -0.5100 0.2303 0.043 Uiso 0.877(3) 1 calc PR B 1 N29A N -0.10655(18) -0.3514(2) 0.34373(12) 0.0288(5) Uani 0.877(3) 1 d PDU B 1 O30A O -0.05018(18) -0.2608(3) 0.35309(15) 0.0504(7) Uani 0.877(3) 1 d PDU B 1 O31A O -0.0764(2) -0.4484(3) 0.36665(16) 0.0426(6) Uani 0.877(3) 1 d PDU B 1 N1'A N -0.8160(2) -0.1823(2) 0.32730(9) 0.0151(4) Uani 0.877(3) 1 d PDU B 1 H2NA H -0.855(2) -0.213(3) 0.3580(14) 0.018 Uiso 0.877(3) 1 d P B 1 C2'A C -0.8479(2) -0.1962(3) 0.26176(10) 0.0157(4) Uani 0.877(3) 1 d PDU B 1 H2'A H -0.9148 -0.2369 0.2430 0.019 Uiso 0.877(3) 1 calc PR B 1 C3'A C -0.7693(3) -0.1428(4) 0.22770(12) 0.0149(4) Uani 0.877(3) 1 d PDU B 1 C4'A C -0.6827(3) -0.0915(4) 0.27486(16) 0.0147(6) Uani 0.877(3) 1 d PDU B 1 C5'A C -0.5834(2) -0.0215(2) 0.27147(13) 0.0172(5) Uani 0.877(3) 1 d PDU B 1 H5'A H -0.5599 -0.0002 0.2305 0.021 Uiso 0.877(3) 1 calc PR B 1 C6'A C -0.5213(2) 0.0153(2) 0.32881(13) 0.0208(5) Uani 0.877(3) 1 d PDU B 1 H6'A H -0.4553 0.0638 0.3271 0.025 Uiso 0.877(3) 1 calc PR B 1 C7'A C -0.5535(2) -0.0175(3) 0.38968(16) 0.0196(6) Uani 0.877(3) 1 d PDU B 1 H7'A H -0.5070 0.0065 0.4282 0.024 Uiso 0.877(3) 1 calc PR B 1 C8'A C -0.6513(3) -0.0838(3) 0.39486(14) 0.0189(6) Uani 0.877(3) 1 d PDU B 1 H8'A H -0.6739 -0.1047 0.4361 0.023 Uiso 0.877(3) 1 calc PR B 1 C9'A C -0.7154(2) -0.1190(2) 0.33665(13) 0.0139(5) Uani 0.877(3) 1 d PDU B 1 S1C S -0.7375(6) -0.0225(6) -0.0752(3) 0.03122(17) Uani 0.123(3) 1 d PU B 2 S2C S -0.7752(7) -0.1701(8) -0.0132(3) 0.0399(16) Uani 0.123(3) 1 d PU B 2 N1C N -0.8583(14) 0.0714(15) 0.1122(11) 0.027(3) Uani 0.123(3) 1 d PDU B 2 H1C H -0.8746 0.1477 0.1113 0.032 Uiso 0.123(3) 1 calc PR B 2 C2C C -0.7444(15) 0.0222(17) 0.1325(13) 0.0155(4) Uani 0.123(3) 1 d PDU B 2 H2C H -0.6963 0.0676 0.1672 0.019 Uiso 0.123(3) 1 calc PR B 2 C3C C -0.7756(15) -0.1063(16) 0.1510(10) 0.0150(4) Uani 0.123(3) 1 d PDU B 2 C4C C -0.8970(13) -0.1253(14) 0.1164(7) 0.024(3) Uani 0.123(3) 1 d PDU B 2 C5C C -0.9583(13) -0.2270(16) 0.1068(8) 0.0273(5) Uani 0.123(3) 1 d PDU B 2 H5C H -0.9259 -0.3003 0.1227 0.033 Uiso 0.123(3) 1 calc PR B 2 C6C C -1.0708(16) -0.224(2) 0.0731(9) 0.0366(6) Uani 0.123(3) 1 d PDU B 2 H6C H -1.1170 -0.2927 0.0647 0.044 Uiso 0.123(3) 1 calc PR B 2 C7C C -1.1068(15) -0.113(2) 0.0538(9) 0.0372(6) Uani 0.123(3) 1 d PDU B 2 H7C H -1.1824 -0.1090 0.0314 0.045 Uiso 0.123(3) 1 calc PR B 2 C8C C -1.0491(13) -0.007(2) 0.0621(9) 0.042(4) Uani 0.123(3) 1 d PDU B 2 H8C H -1.0818 0.0669 0.0472 0.051 Uiso 0.123(3) 1 calc PR B 2 C9C C -0.9370(13) -0.0175(16) 0.0948(9) 0.031(4) Uani 0.123(3) 1 d PDU B 2 C12C C -0.697(2) -0.187(3) 0.1257(14) 0.0154(5) Uani 0.123(3) 1 d PU B 2 H12C H -0.7381 -0.2641 0.1162 0.018 Uiso 0.123(3) 1 calc PR B 2 N10C N -0.690(3) -0.0040(19) 0.0757(14) 0.0187(6) Uani 0.123(3) 1 d PDU B 2 C11C C -0.6772(14) -0.1232(16) 0.0529(11) 0.022(2) Uani 0.123(3) 1 d PDU B 2 C13C C -0.5539(14) -0.1400(13) 0.0367(9) 0.0204(4) Uani 0.123(3) 1 d PDU B 2 N14C N -0.5269(14) -0.0422(15) 0.0012(9) 0.0220(4) Uani 0.123(3) 1 d PDU B 2 C15C C -0.6182(19) 0.038(2) -0.0225(10) 0.031(3) Uani 0.123(3) 1 d PDU B 2 H15C H -0.5843 0.1054 -0.0457 0.037 Uiso 0.123(3) 1 calc PR B 2 C16C C -0.670(3) 0.0885(19) 0.0370(13) 0.0233(6) Uani 0.123(3) 1 d PDU B 2 C17C C -0.4326(17) -0.052(2) -0.0399(10) 0.036(4) Uani 0.123(3) 1 d PDU B 2 H17G H -0.4070 -0.1348 -0.0408 0.054 Uiso 0.123(3) 1 calc PR B 2 H17H H -0.3682 -0.0018 -0.0220 0.054 Uiso 0.123(3) 1 calc PR B 2 H17I H -0.4599 -0.0261 -0.0843 0.054 Uiso 0.123(3) 1 calc PR B 2 O18C O -0.4982(14) -0.2310(12) 0.0475(9) 0.032(3) Uani 0.123(3) 1 d PDU B 2 O19C O -0.693(4) 0.192(2) 0.0459(16) 0.0320(7) Uani 0.123(3) 1 d PDU B 2 O20C O -0.5859(16) -0.2135(15) 0.1558(7) 0.0161(3) Uani 0.123(3) 1 d PDU B 2 C21C C -0.5605(15) -0.3184(16) 0.1805(6) 0.0208(4) Uani 0.123(3) 1 d PDU B 2 O22C O -0.6284(14) -0.3991(13) 0.1722(9) 0.0383(6) Uani 0.123(3) 1 d PDU B 2 C23C C -0.4442(18) -0.332(2) 0.2173(15) 0.0196(4) Uani 0.123(3) 1 d PDU B 2 C24C C -0.3626(17) -0.2496(18) 0.2166(12) 0.0365(6) Uani 0.123(3) 1 d PDU B 2 H24C H -0.3800 -0.1806 0.1909 0.044 Uiso 0.123(3) 1 calc PR B 2 C25C C -0.2558(18) -0.258(2) 0.2503(12) 0.042(4) Uani 0.123(3) 1 d PDU B 2 H25C H -0.2023 -0.1950 0.2490 0.050 Uiso 0.123(3) 1 calc PR B 2 C26C C -0.225(2) -0.3591(16) 0.2863(10) 0.0224(5) Uani 0.123(3) 1 d PDU B 2 C27C C -0.3135(19) -0.441(2) 0.2895(15) 0.0382(7) Uani 0.123(3) 1 d PDU B 2 H27C H -0.2984 -0.5114 0.3143 0.046 Uiso 0.123(3) 1 calc PR B 2 C28C C -0.4193(15) -0.4232(18) 0.2584(9) 0.023(3) Uani 0.123(3) 1 d PDU B 2 H28C H -0.4789 -0.4772 0.2657 0.028 Uiso 0.123(3) 1 calc PR B 2 N29C N -0.1344(15) -0.3574(16) 0.3273(9) 0.0288(5) Uani 0.123(3) 1 d PDU B 2 O30C O -0.0515(14) -0.290(2) 0.3220(11) 0.0504(7) Uani 0.123(3) 1 d PDU B 2 O31C O -0.102(2) -0.450(3) 0.3583(14) 0.0426(6) Uani 0.123(3) 1 d PDU B 2 N1'C N -0.8124(18) -0.195(2) 0.3149(9) 0.0151(4) Uani 0.123(3) 1 d PDU B 2 H1'C H -0.8549 -0.2255 0.3430 0.018 Uiso 0.123(3) 1 calc PR B 2 C2'C C -0.840(2) -0.195(2) 0.2492(10) 0.0157(4) Uani 0.123(3) 1 d PDU B 2 H2'C H -0.9077 -0.2296 0.2273 0.019 Uiso 0.123(3) 1 calc PR B 2 C3'C C -0.761(2) -0.140(3) 0.2192(10) 0.0149(4) Uani 0.123(3) 1 d PDU B 2 C4'C C -0.674(2) -0.103(4) 0.2709(11) 0.0147(6) Uani 0.123(3) 1 d PDU B 2 C5'C C -0.5677(18) -0.046(2) 0.2713(10) 0.0172(5) Uani 0.123(3) 1 d PDU B 2 H5'C H -0.5374 -0.0310 0.2313 0.021 Uiso 0.123(3) 1 calc PR B 2 C6'C C -0.507(2) -0.011(2) 0.3289(10) 0.0208(5) Uani 0.123(3) 1 d PDU B 2 H6'C H -0.4442 0.0429 0.3286 0.025 Uiso 0.123(3) 1 calc PR B 2 C7'C C -0.538(2) -0.054(2) 0.3887(10) 0.028(5) Uani 0.123(3) 1 d PDU B 2 H7'C H -0.4859 -0.0483 0.4274 0.033 Uiso 0.123(3) 1 calc PR B 2 C8'C C -0.645(2) -0.105(3) 0.3901(11) 0.0189(6) Uani 0.123(3) 1 d PDU B 2 H8'C H -0.6756 -0.1172 0.4304 0.023 Uiso 0.123(3) 1 calc PR B 2 C9'C C -0.7085(19) -0.139(2) 0.3309(10) 0.0139(5) Uani 0.123(3) 1 d PDU B 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 0.0184(5) 0.0206(4) 0.0150(3) -0.0001(2) -0.0012(3) 0.0048(3) S2 0.0296(4) 0.0171(4) 0.0155(4) -0.0014(3) -0.0029(2) 0.0097(2) N1 0.0179(7) 0.0077(12) 0.0228(11) 0.0018(9) 0.0039(7) -0.0006(8) C2 0.0171(14) 0.0107(13) 0.0117(17) -0.0048(10) 0.0018(10) 0.0016(9) C3 0.0111(9) 0.0091(11) 0.0129(8) 0.0026(8) 0.0008(7) -0.0017(7) C4 0.0137(10) 0.0142(13) 0.0147(8) -0.0002(10) 0.0011(7) -0.0008(8) C5 0.0169(10) 0.0143(12) 0.0199(7) 0.0015(9) -0.0013(7) 0.0009(8) C6 0.0154(13) 0.033(2) 0.0231(12) -0.0005(15) -0.0037(10) 0.0052(13) C7 0.0179(12) 0.036(2) 0.0254(14) -0.0019(14) -0.0026(9) -0.0011(13) C8 0.0184(11) 0.0231(17) 0.0250(14) -0.0031(13) 0.0048(9) -0.0042(11) C9 0.0182(11) 0.0109(12) 0.0163(11) -0.0023(11) 0.0038(8) -0.0032(9) C12 0.0082(13) 0.0136(8) 0.0189(10) -0.0009(7) -0.0024(10) 0.0002(11) N10 0.0165(11) 0.0099(11) 0.0095(11) -0.0022(7) -0.0006(8) -0.0020(7) C11 0.0180(10) 0.0085(11) 0.0135(10) -0.0038(7) 0.0013(8) -0.0001(8) C13 0.0251(12) 0.0171(9) 0.0136(13) -0.0057(9) 0.0047(10) -0.0081(8) N14 0.0162(10) 0.0129(13) 0.0163(14) -0.0026(9) 0.0048(10) -0.0022(8) C15 0.0123(12) 0.0130(15) 0.0131(15) -0.0002(11) -0.0002(12) -0.0013(9) C16 0.0121(9) 0.0110(14) 0.0142(10) -0.0028(10) 0.0021(6) 0.0044(11) C17 0.0224(12) 0.014(2) 0.0278(15) -0.0043(15) 0.0127(10) -0.0085(13) O18 0.0425(15) 0.0235(8) 0.0329(15) -0.0122(11) 0.0154(11) -0.0201(10) O19 0.0216(11) 0.0066(11) 0.0196(7) -0.0010(9) 0.0065(6) 0.0040(9) O20 0.0112(13) 0.0119(14) 0.0207(12) -0.0064(8) -0.0012(9) 0.0001(10) C21 0.0122(13) 0.0134(11) 0.0160(14) -0.0027(9) -0.0023(9) -0.0020(10) O22 0.0158(12) 0.0201(9) 0.0416(9) -0.0080(7) -0.0034(12) 0.0040(11) C23 0.0151(12) 0.0177(11) 0.0155(16) -0.0025(11) -0.0006(9) 0.0032(9) C24 0.0169(11) 0.0169(12) 0.0207(13) -0.0066(10) -0.0006(9) 0.0009(8) C25 0.0192(9) 0.0231(12) 0.0223(13) -0.0040(10) 0.0018(10) 0.0017(8) C26 0.0109(10) 0.0254(14) 0.0185(14) -0.0040(11) -0.0022(8) -0.0025(9) C27 0.0215(15) 0.0261(14) 0.028(2) -0.0115(13) 0.0011(12) 0.0019(13) C28 0.0176(13) 0.0259(14) 0.0278(18) -0.0112(11) -0.0014(12) 0.0031(12) N29 0.0194(11) 0.0253(14) 0.0261(15) -0.0001(9) -0.0005(9) 0.0026(9) O30 0.0349(14) 0.0373(16) 0.0427(16) -0.0182(12) 0.0064(10) -0.0134(10) O31 0.0173(8) 0.0473(13) 0.0316(14) -0.0057(11) -0.0032(9) 0.0061(8) N1' 0.0220(7) 0.0231(9) 0.0176(6) -0.0035(6) 0.0009(5) 0.0046(6) C2' 0.0169(10) 0.0134(19) 0.0178(8) 0.0004(11) 0.0012(7) 0.0006(11) C3' 0.0148(10) 0.0125(18) 0.0163(7) -0.0020(9) -0.0007(6) 0.0003(10) C4' 0.0186(8) 0.0182(13) 0.0164(7) -0.0033(7) -0.0028(6) 0.0037(9) C5' 0.0178(11) 0.021(2) 0.0204(9) -0.0023(10) -0.0007(8) 0.0040(11) C6' 0.0158(11) 0.0276(16) 0.0260(10) -0.0002(10) -0.0048(8) 0.0010(9) C7' 0.0261(12) 0.0287(16) 0.0230(10) -0.0036(11) -0.0095(8) 0.0006(11) C8' 0.0276(12) 0.0250(17) 0.0197(9) -0.0029(11) -0.0069(8) 0.0018(11) C9' 0.0229(11) 0.017(2) 0.0168(8) -0.0031(9) -0.0022(8) 0.0005(11) S1B 0.026(3) 0.117(6) 0.049(3) 0.049(3) 0.0132(19) 0.013(3) S2B 0.151(7) 0.037(4) 0.023(2) 0.001(2) -0.020(3) 0.039(4) N1B 0.0179(7) 0.0077(12) 0.0228(11) 0.0018(9) 0.0039(7) -0.0006(8) C2B 0.009(5) 0.021(5) 0.010(5) -0.004(5) -0.001(4) -0.010(4) C3B 0.0111(9) 0.0091(11) 0.0129(8) 0.0026(8) 0.0008(7) -0.0017(7) C4B 0.0145(14) 0.0119(16) 0.0173(14) 0.0022(15) -0.0005(13) -0.0016(13) C5B 0.0169(10) 0.0143(12) 0.0199(7) 0.0015(9) -0.0013(7) 0.0009(8) C6B 0.023(6) 0.037(8) 0.031(7) -0.017(7) -0.006(5) 0.000(5) C7B 0.017(5) 0.040(9) 0.036(7) 0.009(7) -0.006(4) -0.001(5) C8B 0.026(5) 0.028(7) 0.033(7) 0.007(6) -0.003(4) -0.016(5) C9B 0.008(4) 0.026(5) 0.029(6) 0.007(6) -0.005(3) -0.003(4) C12B 0.0082(13) 0.0136(8) 0.0189(10) -0.0009(7) -0.0024(10) 0.0002(11) N10B 0.0165(11) 0.0099(11) 0.0095(11) -0.0022(7) -0.0006(8) -0.0020(7) C11B 0.039(6) 0.015(5) 0.033(5) 0.017(4) 0.003(4) 0.004(4) C13B 0.0251(12) 0.0171(9) 0.0136(13) -0.0057(9) 0.0047(10) -0.0081(8) N14B 0.038(6) 0.020(6) 0.024(8) -0.005(4) 0.000(5) -0.013(4) C15B 0.031(8) 0.016(6) 0.009(5) -0.007(4) -0.001(4) -0.002(4) C16B 0.0121(9) 0.0110(14) 0.0142(10) -0.0028(10) 0.0021(6) 0.0044(11) C17B 0.047(9) 0.009(9) 0.053(12) -0.012(7) 0.021(9) -0.005(6) O18B 0.0425(15) 0.0235(8) 0.0329(15) -0.0122(11) 0.0154(11) -0.0201(10) O19B 0.0216(11) 0.0066(11) 0.0196(7) -0.0010(9) 0.0065(6) 0.0040(9) O20B 0.019(6) 0.018(5) 0.040(9) -0.001(5) -0.002(5) -0.010(4) C21B 0.028(7) 0.017(5) 0.028(7) -0.009(4) -0.006(5) -0.001(5) O22B 0.0158(12) 0.0201(9) 0.0416(9) -0.0080(7) -0.0034(12) 0.0040(11) C23B 0.026(5) 0.030(6) 0.019(8) 0.005(5) -0.008(4) -0.003(4) C24B 0.038(6) 0.033(8) 0.037(9) -0.015(6) -0.009(6) 0.008(5) C25B 0.0192(9) 0.0231(12) 0.0223(13) -0.0040(10) 0.0018(10) 0.0017(8) C26B 0.039(6) 0.018(5) 0.028(8) -0.009(5) -0.003(5) 0.009(5) C27B 0.037(7) 0.032(6) 0.030(6) -0.018(4) -0.010(6) 0.006(6) C28B 0.038(7) 0.031(5) 0.029(6) -0.025(4) -0.006(6) 0.008(6) N29B 0.0194(11) 0.0253(14) 0.0261(15) -0.0001(9) -0.0005(9) 0.0026(9) O30B 0.0349(14) 0.0373(16) 0.0427(16) -0.0182(12) 0.0064(10) -0.0134(10) O31B 0.0173(8) 0.0473(13) 0.0316(14) -0.0057(11) -0.0032(9) 0.0061(8) N1'B 0.0220(7) 0.0231(9) 0.0176(6) -0.0035(6) 0.0009(5) 0.0046(6) C2'B 0.0169(10) 0.0134(19) 0.0178(8) 0.0004(11) 0.0012(7) 0.0006(11) C3'B 0.0148(10) 0.0125(18) 0.0163(7) -0.0020(9) -0.0007(6) 0.0003(10) C4'B 0.0186(8) 0.0182(13) 0.0164(7) -0.0033(7) -0.0028(6) 0.0037(9) C5'B 0.0178(11) 0.021(2) 0.0204(9) -0.0023(10) -0.0007(8) 0.0040(11) C6'B 0.0158(11) 0.0276(16) 0.0260(10) -0.0002(10) -0.0048(8) 0.0010(9) C7'B 0.0261(12) 0.0287(16) 0.0230(10) -0.0036(11) -0.0095(8) 0.0006(11) C8'B 0.0276(12) 0.0250(17) 0.0197(9) -0.0029(11) -0.0069(8) 0.0018(11) C9'B 0.0229(11) 0.017(2) 0.0168(8) -0.0031(9) -0.0022(8) 0.0005(11) S1A 0.0358(4) 0.0397(3) 0.0168(2) 0.0042(2) -0.0028(2) 0.0114(3) S2A 0.0334(4) 0.0309(3) 0.0149(2) -0.0037(2) -0.0037(3) 0.0002(3) N1A 0.0224(11) 0.0243(13) 0.0331(11) 0.0040(11) -0.0010(9) 0.0081(10) C2A 0.0201(10) 0.0141(11) 0.0121(6) 0.0018(9) 0.0007(7) 0.0027(7) C3A 0.0179(7) 0.0128(11) 0.0135(7) -0.0005(8) -0.0023(5) 0.0017(8) C4A 0.0163(8) 0.0301(14) 0.0129(9) -0.0013(9) -0.0042(6) 0.0029(9) C5A 0.0257(10) 0.0323(14) 0.0217(9) -0.0015(9) -0.0061(7) -0.0011(9) C6A 0.0305(12) 0.0470(17) 0.0296(12) -0.0026(12) -0.0087(9) -0.0122(12) C7A 0.0207(10) 0.0572(19) 0.0306(11) -0.0024(13) -0.0102(8) -0.0013(12) C8A 0.0221(11) 0.0481(17) 0.0253(11) 0.0059(12) -0.0095(9) 0.0080(11) C9A 0.0202(9) 0.0312(14) 0.0161(9) -0.0005(10) -0.0019(7) 0.0053(9) C12A 0.0171(13) 0.0148(13) 0.0139(7) -0.0032(8) 0.0000(8) 0.0060(7) N10A 0.0264(13) 0.0154(8) 0.0146(11) 0.0003(6) 0.0034(10) 0.0073(7) C11A 0.0220(10) 0.0154(9) 0.0105(8) -0.0003(7) -0.0015(7) 0.0054(8) C13A 0.0251(11) 0.0183(9) 0.0174(10) -0.0019(7) 0.0017(7) 0.0044(8) N14A 0.0254(10) 0.0187(8) 0.0226(10) 0.0038(7) 0.0056(7) 0.0067(8) C15A 0.0339(13) 0.0177(10) 0.0165(10) 0.0018(8) 0.0070(9) 0.0086(9) C16A 0.0352(16) 0.0186(10) 0.0169(11) 0.0050(7) 0.0066(10) 0.0116(9) C17A 0.0332(13) 0.0311(14) 0.0427(15) 0.0111(12) 0.0204(12) 0.0095(12) O18A 0.0279(9) 0.0217(9) 0.0258(9) 0.0014(7) 0.0067(7) 0.0088(8) O19A 0.055(2) 0.0178(9) 0.0253(14) 0.0055(8) 0.0140(12) 0.0140(8) O20A 0.0200(7) 0.0151(6) 0.0119(8) -0.0010(7) -0.0034(7) 0.0033(5) C21A 0.0253(12) 0.0169(9) 0.0185(7) 0.0003(6) -0.0052(7) 0.0042(8) O22A 0.0449(12) 0.0125(8) 0.0502(12) -0.0011(7) -0.0256(10) 0.0027(8) C23A 0.0203(12) 0.0196(9) 0.0176(12) 0.0018(7) -0.0029(8) 0.0018(8) C24A 0.0313(11) 0.0141(11) 0.0590(19) -0.0059(11) -0.0163(12) 0.0030(9) C25A 0.0257(12) 0.0229(12) 0.067(2) -0.0035(13) -0.0151(13) 0.0004(9) C26A 0.0200(9) 0.0270(12) 0.0202(12) -0.0022(8) 0.0018(10) 0.0020(8) C27A 0.0328(15) 0.0259(12) 0.0497(15) 0.0103(10) -0.0221(15) 0.0016(13) C28A 0.0320(15) 0.0191(12) 0.0512(18) 0.0078(12) -0.0212(13) 0.0016(11) N29A 0.0126(9) 0.0422(12) 0.0302(12) 0.0050(9) -0.0030(7) 0.0038(8) O30A 0.0203(8) 0.0587(16) 0.0683(17) 0.0102(13) -0.0113(10) -0.0093(9) O31A 0.0340(15) 0.0481(11) 0.0402(13) 0.0038(10) -0.0192(10) 0.0134(12) N1'A 0.0182(6) 0.0167(9) 0.0101(10) -0.0023(7) -0.0002(7) -0.0009(6) C2'A 0.0168(8) 0.0175(8) 0.0126(11) -0.0015(9) 0.0010(8) 0.0009(6) C3'A 0.0163(9) 0.0165(8) 0.0118(10) -0.0013(9) 0.0012(7) -0.0005(7) C4'A 0.0165(9) 0.0134(13) 0.0135(8) 0.0001(7) -0.0010(6) 0.0010(9) C5'A 0.0185(10) 0.0149(13) 0.0179(7) 0.0009(8) 0.0016(7) 0.0023(8) C6'A 0.0220(11) 0.0193(14) 0.0201(7) -0.0023(9) -0.0013(7) -0.0013(9) C7'A 0.0200(10) 0.0186(14) 0.0186(9) -0.0025(10) -0.0044(7) -0.0006(9) C8'A 0.0244(9) 0.0201(16) 0.0115(8) -0.0024(8) -0.0008(6) -0.0016(10) C9'A 0.0170(8) 0.0107(13) 0.0136(8) -0.0015(7) -0.0004(6) 0.0015(8) S1C 0.0358(4) 0.0397(3) 0.0168(2) 0.0042(2) -0.0028(2) 0.0114(3) S2C 0.030(3) 0.065(4) 0.022(2) -0.018(2) -0.006(2) -0.008(3) N1C 0.015(5) 0.020(7) 0.042(9) 0.015(7) -0.009(5) 0.000(5) C2C 0.0201(10) 0.0141(11) 0.0121(6) 0.0018(9) 0.0007(7) 0.0027(7) C3C 0.0179(7) 0.0128(11) 0.0135(7) -0.0005(8) -0.0023(5) 0.0017(8) C4C 0.035(5) 0.014(6) 0.019(6) 0.006(6) -0.013(5) -0.003(5) C5C 0.0257(10) 0.0323(14) 0.0217(9) -0.0015(9) -0.0061(7) -0.0011(9) C6C 0.0305(12) 0.0470(17) 0.0296(12) -0.0026(12) -0.0087(9) -0.0122(12) C7C 0.0207(10) 0.0572(19) 0.0306(11) -0.0024(13) -0.0102(8) -0.0013(12) C8C 0.024(7) 0.059(7) 0.039(9) 0.012(10) -0.014(6) -0.005(7) C9C 0.035(6) 0.024(7) 0.030(8) 0.013(8) -0.015(6) 0.000(6) C12C 0.0171(13) 0.0148(13) 0.0139(7) -0.0032(8) 0.0000(8) 0.0060(7) N10C 0.0264(13) 0.0154(8) 0.0146(11) 0.0003(6) 0.0034(10) 0.0073(7) C11C 0.026(6) 0.013(5) 0.027(5) 0.002(4) 0.002(4) -0.005(5) C13C 0.0251(11) 0.0183(9) 0.0174(10) -0.0019(7) 0.0017(7) 0.0044(8) N14C 0.0254(10) 0.0187(8) 0.0226(10) 0.0038(7) 0.0056(7) 0.0067(8) C15C 0.035(8) 0.035(7) 0.024(7) 0.009(5) 0.007(6) 0.008(5) C16C 0.0352(16) 0.0186(10) 0.0169(11) 0.0050(7) 0.0066(10) 0.0116(9) C17C 0.031(8) 0.041(11) 0.036(9) -0.009(8) 0.003(6) -0.008(7) O18C 0.030(7) 0.023(6) 0.047(9) -0.004(6) 0.021(7) -0.001(5) O19C 0.055(2) 0.0178(9) 0.0253(14) 0.0055(8) 0.0140(12) 0.0140(8) O20C 0.0200(7) 0.0151(6) 0.0119(8) -0.0010(7) -0.0034(7) 0.0033(5) C21C 0.0253(12) 0.0169(9) 0.0185(7) 0.0003(6) -0.0052(7) 0.0042(8) O22C 0.0449(12) 0.0125(8) 0.0502(12) -0.0011(7) -0.0256(10) 0.0027(8) C23C 0.0203(12) 0.0196(9) 0.0176(12) 0.0018(7) -0.0029(8) 0.0018(8) C24C 0.0313(11) 0.0141(11) 0.0590(19) -0.0059(11) -0.0163(12) 0.0030(9) C25C 0.036(7) 0.038(9) 0.049(10) 0.018(8) -0.007(7) -0.013(7) C26C 0.0200(9) 0.0270(12) 0.0202(12) -0.0022(8) 0.0018(10) 0.0020(8) C27C 0.0328(15) 0.0259(12) 0.0497(15) 0.0103(10) -0.0221(15) 0.0016(13) C28C 0.016(6) 0.023(7) 0.030(7) 0.002(5) 0.002(5) 0.010(5) N29C 0.0126(9) 0.0422(12) 0.0302(12) 0.0050(9) -0.0030(7) 0.0038(8) O30C 0.0203(8) 0.0587(16) 0.0683(17) 0.0102(13) -0.0113(10) -0.0093(9) O31C 0.0340(15) 0.0481(11) 0.0402(13) 0.0038(10) -0.0192(10) 0.0134(12) N1'C 0.0182(6) 0.0167(9) 0.0101(10) -0.0023(7) -0.0002(7) -0.0009(6) C2'C 0.0168(8) 0.0175(8) 0.0126(11) -0.0015(9) 0.0010(8) 0.0009(6) C3'C 0.0163(9) 0.0165(8) 0.0118(10) -0.0013(9) 0.0012(7) -0.0005(7) C4'C 0.0165(9) 0.0134(13) 0.0135(8) 0.0001(7) -0.0010(6) 0.0010(9) C5'C 0.0185(10) 0.0149(13) 0.0179(7) 0.0009(8) 0.0016(7) 0.0023(8) C6'C 0.0220(11) 0.0193(14) 0.0201(7) -0.0023(9) -0.0013(7) -0.0013(9) C7'C 0.041(9) 0.025(11) 0.013(5) 0.008(7) -0.014(6) -0.003(8) C8'C 0.0244(9) 0.0201(16) 0.0115(8) -0.0024(8) -0.0008(6) -0.0016(10) C9'C 0.0170(8) 0.0107(13) 0.0136(8) -0.0015(7) -0.0004(6) 0.0015(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 C15 1.851(6) . ? S1 S2 2.0727(15) . ? S2 C11 1.866(3) . ? N1 C9 1.401(4) . ? N1 C2 1.441(5) . ? C2 N10 1.486(8) . ? C2 C3 1.555(4) . ? C3 C3' 1.502(6) . ? C3 C4 1.527(3) . ? C3 C12 1.572(4) . ? C4 C5 1.384(3) . ? C4 C9 1.390(4) . ? C5 C6 1.410(4) . ? C6 C7 1.387(5) . ? C7 C8 1.391(5) . ? C8 C9 1.388(4) . ? C12 O20 1.440(4) . ? C12 C11 1.550(4) . ? N10 C16 1.355(3) . ? N10 C11 1.447(4) . ? C11 C13 1.532(3) . ? C13 O18 1.222(3) . ? C13 N14 1.353(4) . ? N14 C15 1.439(4) . ? N14 C17 1.465(3) . ? C15 C16 1.523(4) . ? C16 O19 1.223(3) . ? O20 C21 1.358(5) . ? C21 O22 1.209(4) . ? C21 C23 1.484(4) . ? C23 C28 1.391(4) . ? C23 C24 1.396(4) . ? C24 C25 1.393(3) . ? C25 C26 1.389(4) . ? C26 C27 1.394(4) . ? C26 N29 1.472(4) . ? C27 C28 1.382(3) . ? N29 O31 1.232(4) . ? N29 O30 1.237(4) . ? N1' C2' 1.371(4) . ? N1' C9' 1.372(4) . ? C2' C3' 1.370(4) . ? C3' C4' 1.450(4) . ? C4' C5' 1.407(4) . ? C4' C9' 1.418(4) . ? C5' C6' 1.385(4) . ? C6' C7' 1.411(4) . ? C7' C8' 1.384(4) . ? C8' C9' 1.402(3) . ? S1B C15B 1.85(4) . ? S1B S2B 2.379(13) . ? S2B C11B 1.91(2) . ? N1B C9B 1.374(13) . ? N1B C2B 1.441(14) . ? C2B N10B 1.50(4) . ? C2B C3B 1.538(15) . ? C3B C12B 1.43(2) . ? C3B C4B 1.525(13) . ? C3B C3'B 1.57(3) . ? C4B C9B 1.347(13) . ? C4B C5B 1.365(12) . ? C5B C6B 1.405(14) . ? C6B C7B 1.354(15) . ? C7B C8B 1.386(15) . ? C8B C9B 1.420(13) . ? C12B C11B 1.35(3) . ? C12B O20B 1.40(2) . ? N10B C16B 1.308(13) . ? N10B C11B 1.460(14) . ? C11B C13B 1.516(14) . ? C13B O18B 1.210(13) . ? C13B N14B 1.339(14) . ? N14B C15B 1.436(14) . ? N14B C17B 1.459(15) . ? C15B C16B 1.549(14) . ? C16B O19B 1.230(14) . ? O20B C21B 1.37(3) . ? C21B O22B 1.23(3) . ? C21B C23B 1.37(2) . ? C23B C28B 1.395(13) . ? C23B C24B 1.397(13) . ? C24B C25B 1.364(12) . ? C25B C26B 1.387(12) . ? C26B C27B 1.387(13) . ? C26B N29B 1.41(2) . ? C27B C28B 1.361(13) . ? N29B O31B 1.15(2) . ? N29B O30B 1.23(2) . ? N1'B C9'B 1.374(14) . ? N1'B C2'B 1.377(15) . ? C2'B C3'B 1.363(15) . ? C3'B C4'B 1.443(14) . ? C4'B C5'B 1.404(14) . ? C4'B C9'B 1.420(14) . ? C5'B C6'B 1.356(14) . ? C6'B C7'B 1.390(13) . ? C7'B C8'B 1.384(14) . ? C8'B C9'B 1.403(13) . ? S1A C15A 1.881(3) . ? S1A S2A 2.0862(11) . ? S2A C11A 1.883(2) . ? N1A C9A 1.378(4) . ? N1A C2A 1.440(3) . ? C2A N10A 1.486(4) . ? C2A C3A 1.565(3) . ? C3A C4A 1.513(3) . ? C3A C3'A 1.525(4) . ? C3A C12A 1.571(3) . ? C4A C5A 1.377(4) . ? C4A C9A 1.391(4) . ? C5A C6A 1.406(3) . ? C6A C7A 1.387(5) . ? C7A C8A 1.379(5) . ? C8A C9A 1.399(3) . ? C12A O20A 1.443(3) . ? C12A C11A 1.532(4) . ? N10A C16A 1.349(3) . ? N10A C11A 1.427(3) . ? C11A C13A 1.540(3) . ? C13A O18A 1.216(3) . ? C13A N14A 1.351(3) . ? N14A C15A 1.431(3) . ? N14A C17A 1.460(3) . ? C15A C16A 1.518(3) . ? C16A O19A 1.223(3) . ? O20A C21A 1.348(3) . ? C21A O22A 1.206(3) . ? C21A C23A 1.498(3) . ? C23A C28A 1.382(4) . ? C23A C24A 1.389(4) . ? C24A C25A 1.394(3) . ? C25A C26A 1.368(4) . ? C26A C27A 1.371(4) . ? C26A N29A 1.482(3) . ? C27A C28A 1.394(3) . ? N29A O30A 1.218(4) . ? N29A O31A 1.227(4) . ? N1'A C2'A 1.370(2) . ? N1'A C9'A 1.370(3) . ? C2'A C3'A 1.361(3) . ? C3'A C4'A 1.442(3) . ? C4'A C9'A 1.408(3) . ? C4'A C5'A 1.411(3) . ? C5'A C6'A 1.379(3) . ? C6'A C7'A 1.403(3) . ? C7'A C8'A 1.380(3) . ? C8'A C9'A 1.398(3) . ? S1C C15C 1.80(3) . ? S1C S2C 2.175(10) . ? S2C C11C 1.76(2) . ? N1C C9C 1.380(15) . ? N1C C2C 1.459(15) . ? C2C N10C 1.43(4) . ? C2C C3C 1.552(16) . ? C3C C12C 1.44(3) . ? C3C C3'C 1.45(3) . ? C3C C4C 1.528(15) . ? C4C C5C 1.353(15) . ? C4C C9C 1.359(15) . ? C5C C6C 1.416(15) . ? C6C C7C 1.358(17) . ? C7C C8C 1.379(17) . ? C8C C9C 1.408(14) . ? C12C O20C 1.40(3) . ? C12C C11C 1.71(4) . ? N10C C16C 1.351(16) . ? N10C C11C 1.438(16) . ? C11C C13C 1.530(15) . ? C13C O18C 1.220(14) . ? C13C N14C 1.380(14) . ? N14C C15C 1.442(15) . ? N14C C17C 1.472(15) . ? C15C C16C 1.540(16) . ? C16C O19C 1.216(15) . ? O20C C21C 1.308(15) . ? C21C O22C 1.207(15) . ? C21C C23C 1.486(16) . ? C23C C24C 1.33(2) . ? C23C C28C 1.34(2) . ? C24C C25C 1.36(2) . ? C25C C26C 1.38(2) . ? C26C N29C 1.28(3) . ? C26C C27C 1.39(2) . ? C27C C28C 1.34(2) . ? N29C O30C 1.25(2) . ? N29C O31C 1.26(2) . ? N1'C C2'C 1.358(15) . ? N1'C C9'C 1.371(15) . ? C2'C C3'C 1.327(16) . ? C3'C C4'C 1.446(15) . ? C4'C C5'C 1.398(15) . ? C4'C C9'C 1.409(15) . ? C5'C C6'C 1.371(16) . ? C6'C C7'C 1.415(16) . ? C7'C C8'C 1.383(16) . ? C8'C C9'C 1.406(15) . ? 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 C15 S1 S2 98.62(16) . . ? C11 S2 S1 97.68(10) . . ? C9 N1 C2 107.8(3) . . ? N1 C2 N10 115.4(4) . . ? N1 C2 C3 104.9(3) . . ? N10 C2 C3 103.8(4) . . ? C3' C3 C4 113.0(3) . . ? C3' C3 C2 113.7(4) . . ? C4 C3 C2 100.1(2) . . ? C3' C3 C12 113.7(3) . . ? C4 C3 C12 110.4(2) . . ? C2 C3 C12 104.7(4) . . ? C5 C4 C9 120.5(2) . . ? C5 C4 C3 130.5(2) . . ? C9 C4 C3 109.0(2) . . ? C4 C5 C6 119.1(3) . . ? C7 C6 C5 119.2(3) . . ? C6 C7 C8 122.0(3) . . ? C9 C8 C7 117.8(3) . . ? C8 C9 C4 121.3(3) . . ? C8 C9 N1 128.3(3) . . ? C4 C9 N1 110.3(2) . . ? O20 C12 C11 105.1(3) . . ? O20 C12 C3 109.3(3) . . ? C11 C12 C3 105.5(3) . . ? C16 N10 C11 119.6(3) . . ? C16 N10 C2 124.8(3) . . ? C11 N10 C2 115.2(3) . . ? N10 C11 C13 112.1(3) . . ? N10 C11 C12 104.0(3) . . ? C13 C11 C12 118.0(2) . . ? N10 C11 S2 110.99(19) . . ? C13 C11 S2 102.1(2) . . ? C12 C11 S2 109.8(2) . . ? O18 C13 N14 125.4(3) . . ? O18 C13 C11 122.6(3) . . ? N14 C13 C11 111.9(2) . . ? C13 N14 C15 117.6(3) . . ? C13 N14 C17 121.9(3) . . ? C15 N14 C17 118.0(3) . . ? N14 C15 C16 111.0(3) . . ? N14 C15 S1 111.6(4) . . ? C16 C15 S1 105.7(3) . . ? O19 C16 N10 124.9(3) . . ? O19 C16 C15 124.4(3) . . ? N10 C16 C15 110.5(3) . . ? C21 O20 C12 115.9(4) . . ? O22 C21 O20 123.9(3) . . ? O22 C21 C23 124.1(3) . . ? O20 C21 C23 111.9(3) . . ? C28 C23 C24 120.4(3) . . ? C28 C23 C21 117.6(3) . . ? C24 C23 C21 122.0(3) . . ? C25 C24 C23 120.1(3) . . ? C26 C25 C24 118.0(2) . . ? C25 C26 C27 122.9(3) . . ? C25 C26 N29 118.5(3) . . ? C27 C26 N29 118.6(3) . . ? C28 C27 C26 117.9(3) . . ? C27 C28 C23 120.6(3) . . ? O31 N29 O30 121.2(3) . . ? O31 N29 C26 118.0(3) . . ? O30 N29 C26 120.8(3) . . ? C2' N1' C9' 108.9(4) . . ? C3' C2' N1' 110.3(3) . . ? C2' C3' C4' 106.6(3) . . ? C2' C3' C3 125.0(4) . . ? C4' C3' C3 128.4(4) . . ? C5' C4' C9' 118.7(4) . . ? C5' C4' C3' 135.3(4) . . ? C9' C4' C3' 106.0(3) . . ? C6' C5' C4' 119.3(3) . . ? C5' C6' C7' 120.8(3) . . ? C8' C7' C6' 121.4(2) . . ? C7' C8' C9' 117.5(3) . . ? N1' C9' C8' 129.5(4) . . ? N1' C9' C4' 108.3(3) . . ? C8' C9' C4' 122.3(3) . . ? C15B S1B S2B 91.3(9) . . ? C11B S2B S1B 98.3(6) . . ? C9B N1B C2B 109.1(12) . . ? N1B C2B N10B 111(2) . . ? N1B C2B C3B 108.6(11) . . ? N10B C2B C3B 93.9(18) . . ? C12B C3B C4B 121.7(13) . . ? C12B C3B C2B 111.2(17) . . ? C4B C3B C2B 97.9(10) . . ? C12B C3B C3'B 112.4(15) . . ? C4B C3B C3'B 107.1(14) . . ? C2B C3B C3'B 104.4(18) . . ? C9B C4B C5B 117.2(11) . . ? C9B C4B C3B 113.5(10) . . ? C5B C4B C3B 129.2(11) . . ? C4B C5B C6B 118.3(12) . . ? C7B C6B C5B 122.5(15) . . ? C6B C7B C8B 121.8(13) . . ? C7B C8B C9B 112.5(13) . . ? C4B C9B N1B 109.7(10) . . ? C4B C9B C8B 127.6(12) . . ? N1B C9B C8B 122.7(13) . . ? C11B C12B O20B 114.2(18) . . ? C11B C12B C3B 103.3(15) . . ? O20B C12B C3B 116.2(19) . . ? C16B N10B C11B 120.9(14) . . ? C16B N10B C2B 122.1(14) . . ? C11B N10B C2B 113.0(14) . . ? C12B C11B N10B 105.2(15) . . ? C12B C11B C13B 117.2(14) . . ? N10B C11B C13B 106.4(13) . . ? C12B C11B S2B 114.7(13) . . ? N10B C11B S2B 111.2(13) . . ? C13B C11B S2B 102.1(12) . . ? O18B C13B N14B 123.0(14) . . ? O18B C13B C11B 121.0(14) . . ? N14B C13B C11B 115.5(12) . . ? C13B N14B C15B 119.4(16) . . ? C13B N14B C17B 118.4(15) . . ? C15B N14B C17B 119.9(16) . . ? N14B C15B C16B 113.0(15) . . ? N14B C15B S1B 111(2) . . ? C16B C15B S1B 104.2(19) . . ? O19B C16B N10B 126.0(17) . . ? O19B C16B C15B 120.0(16) . . ? N10B C16B C15B 112.7(14) . . ? C21B O20B C12B 125(2) . . ? O22B C21B C23B 134.4(17) . . ? O22B C21B O20B 111.8(17) . . ? C23B C21B O20B 113.9(18) . . ? C21B C23B C28B 117.3(15) . . ? C21B C23B C24B 122.0(15) . . ? C28B C23B C24B 120.1(14) . . ? C25B C24B C23B 117.1(12) . . ? C24B C25B C26B 123.8(12) . . ? C27B C26B C25B 117.6(14) . . ? C27B C26B N29B 122.5(14) . . ? C25B C26B N29B 119.6(14) . . ? C28B C27B C26B 120.4(14) . . ? C27B C28B C23B 120.6(14) . . ? O31B N29B O30B 134.5(17) . . ? O31B N29B C26B 125.3(17) . . ? O30B N29B C26B 99.3(15) . . ? C9'B N1'B C2'B 109.7(15) . . ? C3'B C2'B N1'B 109.7(15) . . ? C2'B C3'B C4'B 106.6(14) . . ? C2'B C3'B C3B 125.8(17) . . ? C4'B C3'B C3B 127.6(18) . . ? C5'B C4'B C9'B 118.2(15) . . ? C5'B C4'B C3'B 134.7(16) . . ? C9'B C4'B C3'B 107.0(12) . . ? C6'B C5'B C4'B 118.7(16) . . ? C5'B C6'B C7'B 123.2(13) . . ? C8'B C7'B C6'B 119.9(12) . . ? C7'B C8'B C9'B 117.9(14) . . ? N1'B C9'B C8'B 130.6(17) . . ? N1'B C9'B C4'B 106.8(13) . . ? C8'B C9'B C4'B 121.5(15) . . ? C15A S1A S2A 97.86(9) . . ? C11A S2A S1A 97.04(9) . . ? C9A N1A C2A 110.7(2) . . ? N1A C2A N10A 115.5(3) . . ? N1A C2A C3A 105.12(19) . . ? N10A C2A C3A 102.6(2) . . ? C4A C3A C3'A 111.0(2) . . ? C4A C3A C2A 101.69(18) . . ? C3'A C3A C2A 110.6(2) . . ? C4A C3A C12A 110.86(19) . . ? C3'A C3A C12A 115.1(2) . . ? C2A C3A C12A 106.5(2) . . ? C5A C4A C9A 121.7(2) . . ? C5A C4A C3A 128.8(2) . . ? C9A C4A C3A 109.5(2) . . ? C4A C5A C6A 118.3(3) . . ? C7A C6A C5A 119.9(3) . . ? C8A C7A C6A 121.7(2) . . ? C7A C8A C9A 118.5(3) . . ? N1A C9A C4A 110.68(19) . . ? N1A C9A C8A 129.3(3) . . ? C4A C9A C8A 119.9(3) . . ? O20A C12A C11A 108.9(2) . . ? O20A C12A C3A 109.3(2) . . ? C11A C12A C3A 104.67(19) . . ? C16A N10A C11A 119.3(3) . . ? C16A N10A C2A 123.9(2) . . ? C11A N10A C2A 115.5(3) . . ? N10A C11A C12A 105.1(2) . . ? N10A C11A C13A 111.9(2) . . ? C12A C11A C13A 117.03(18) . . ? N10A C11A S2A 112.2(2) . . ? C12A C11A S2A 108.65(19) . . ? C13A C11A S2A 102.05(14) . . ? O18A C13A N14A 124.3(2) . . ? O18A C13A C11A 123.8(2) . . ? N14A C13A C11A 111.79(19) . . ? C13A N14A C15A 117.9(2) . . ? C13A N14A C17A 121.3(2) . . ? C15A N14A C17A 119.9(2) . . ? N14A C15A C16A 112.3(2) . . ? N14A C15A S1A 111.13(18) . . ? C16A C15A S1A 104.3(2) . . ? O19A C16A N10A 124.1(3) . . ? O19A C16A C15A 124.7(3) . . ? N10A C16A C15A 111.1(2) . . ? C21A O20A C12A 115.44(19) . . ? O22A C21A O20A 124.01(19) . . ? O22A C21A C23A 123.7(2) . . ? O20A C21A C23A 112.3(2) . . ? C28A C23A C24A 121.3(2) . . ? C28A C23A C21A 117.0(2) . . ? C24A C23A C21A 121.6(2) . . ? C23A C24A C25A 119.2(2) . . ? C26A C25A C24A 118.3(3) . . ? C25A C26A C27A 123.4(3) . . ? C25A C26A N29A 119.0(2) . . ? C27A C26A N29A 117.7(2) . . ? C26A C27A C28A 118.5(3) . . ? C23A C28A C27A 119.2(3) . . ? O30A N29A O31A 124.1(2) . . ? O30A N29A C26A 117.4(2) . . ? O31A N29A C26A 118.5(2) . . ? C2'A N1'A C9'A 109.23(19) . . ? C3'A C2'A N1'A 109.7(2) . . ? C2'A C3'A C4'A 107.0(2) . . ? C2'A C3'A C3A 126.8(2) . . ? C4'A C3'A C3A 126.2(2) . . ? C9'A C4'A C5'A 118.6(2) . . ? C9'A C4'A C3'A 106.3(2) . . ? C5'A C4'A C3'A 135.0(3) . . ? C6'A C5'A C4'A 118.7(2) . . ? C5'A C6'A C7'A 121.4(2) . . ? C8'A C7'A C6'A 121.6(3) . . ? C7'A C8'A C9'A 116.9(3) . . ? N1'A C9'A C8'A 129.4(2) . . ? N1'A C9'A C4'A 107.83(19) . . ? C8'A C9'A C4'A 122.8(2) . . ? C15C S1C S2C 97.6(7) . . ? C11C S2C S1C 93.9(7) . . ? C9C N1C C2C 111.0(13) . . ? N10C C2C N1C 109(2) . . ? N10C C2C C3C 98.6(18) . . ? N1C C2C C3C 101.1(12) . . ? C12C C3C C3'C 100(2) . . ? C12C C3C C4C 109.9(16) . . ? C3'C C3C C4C 114.8(15) . . ? C12C C3C C2C 109(2) . . ? C3'C C3C C2C 119(2) . . ? C4C C3C C2C 104.4(12) . . ? C5C C4C C9C 123.6(13) . . ? C5C C4C C3C 129.4(14) . . ? C9C C4C C3C 107.1(11) . . ? C4C C5C C6C 119.7(15) . . ? C7C C6C C5C 114.0(15) . . ? C6C C7C C8C 129.1(15) . . ? C7C C8C C9C 113.5(16) . . ? C4C C9C N1C 111.7(11) . . ? C4C C9C C8C 120.0(15) . . ? N1C C9C C8C 128.2(15) . . ? O20C C12C C3C 125(2) . . ? O20C C12C C11C 105.6(19) . . ? C3C C12C C11C 102.1(18) . . ? C16C N10C C2C 116.8(17) . . ? C16C N10C C11C 119.7(18) . . ? C2C N10C C11C 122.4(19) . . ? N10C C11C C13C 109.0(17) . . ? N10C C11C C12C 94.4(17) . . ? C13C C11C C12C 111.6(15) . . ? N10C C11C S2C 117(2) . . ? C13C C11C S2C 109.8(13) . . ? C12C C11C S2C 114.5(14) . . ? O18C C13C N14C 128.2(14) . . ? O18C C13C C11C 124.0(14) . . ? N14C C13C C11C 107.3(12) . . ? C13C N14C C15C 118.5(15) . . ? C13C N14C C17C 118.6(14) . . ? C15C N14C C17C 115.2(15) . . ? N14C C15C C16C 107.8(15) . . ? N14C C15C S1C 117.1(17) . . ? C16C C15C S1C 105.8(18) . . ? O19C C16C N10C 126(2) . . ? O19C C16C C15C 126(2) . . ? N10C C16C C15C 107.5(15) . . ? C21C O20C C12C 121(2) . . ? O22C C21C O20C 120.7(16) . . ? O22C C21C C23C 122.9(16) . . ? O20C C21C C23C 116.4(15) . . ? C24C C23C C28C 115.9(18) . . ? C24C C23C C21C 122.6(16) . . ? C28C C23C C21C 121.3(16) . . ? C23C C24C C25C 124.2(18) . . ? C24C C25C C26C 119.8(19) . . ? N29C C26C C25C 119.0(16) . . ? N29C C26C C27C 122.9(17) . . ? C25C C26C C27C 115(2) . . ? C28C C27C C26C 122(2) . . ? C27C C28C C23C 122.5(19) . . ? O30C N29C O31C 111(2) . . ? O30C N29C C26C 123.1(15) . . ? O31C N29C C26C 120.0(15) . . ? C2'C N1'C C9'C 110.0(15) . . ? C3'C C2'C N1'C 111.6(16) . . ? C2'C C3'C C4'C 104.9(15) . . ? C2'C C3'C C3C 124.2(18) . . ? C4'C C3'C C3C 130(2) . . ? C5'C C4'C C9'C 118.4(16) . . ? C5'C C4'C C3'C 133.0(18) . . ? C9'C C4'C C3'C 108.5(13) . . ? C6'C C5'C C4'C 120.5(18) . . ? C5'C C6'C C7'C 119.9(18) . . ? C8'C C7'C C6'C 119.2(17) . . ? C7'C C8'C C9'C 118.8(17) . . ? N1'C C9'C C8'C 134.1(17) . . ? N1'C C9'C C4'C 104.9(13) . . ? C8'C C9'C C4'C 120.6(16) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.032 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.071 _database_code_depnum_ccdc_archive 'CCDC 933938'