# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'Thiourea.cif' _publ_contact_author_name 'Dr. Gopal Das' _publ_contact_author_address ;Department of Chemistry Indian Institute of Technology Guwahati Assam 781039 India ; _publ_contact_author_email gdas@iitg.ernet.in _publ_contact_author_phone 00913612582313 _publ_contact_author_fax 00913612582349 loop_ _publ_author_name _publ_author_address S.Day ;Department of Chemistry Indian Institute of Technology Guwahati Assam 781039 India ; G.Das '' data_Thiourea _database_code_depnum_ccdc_archive 'CCDC 796387' #TrackingRef 'Thiourea.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H37 N11 O7 S3' _chemical_formula_weight 759.92 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3675(5) _cell_length_b 10.4400(6) _cell_length_c 19.5297(11) _cell_angle_alpha 94.671(4) _cell_angle_beta 92.962(4) _cell_angle_gamma 110.626(3) _cell_volume 1774.95(18) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6337 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 22.42 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.888 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and onega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24704 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.34 _reflns_number_total 8599 _reflns_number_gt 6935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.3300P)^2^+0.1000P] 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 ? _refine_ls_extinction_method none _refine_ls_number_reflns 8856 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1576 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.2445 _refine_ls_wR_factor_gt 0.2071 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S3 S -0.14508(17) 0.77827(15) 0.48095(8) 0.0548(5) Uani 1 1 d . . . S2 S 0.34330(18) 0.77942(16) 0.49701(8) 0.0596(5) Uani 1 1 d . . . S1 S 0.3536(2) 0.70343(18) 0.11976(9) 0.0808(7) Uani 1 1 d . . . N1 N 0.1256(5) 0.4895(4) 0.3409(2) 0.0464(10) Uani 1 1 d . . . C2 C 0.1618(8) 0.5420(6) 0.2230(3) 0.0578(15) Uani 1 1 d . . . H2A H 0.1413 0.6270 0.2265 0.069 Uiso 1 1 calc R . . H2B H 0.2687 0.5639 0.2383 0.069 Uiso 1 1 calc R . . C1 C 0.0624(7) 0.4448(6) 0.2695(3) 0.0548(14) Uani 1 1 d . . . H1A H -0.0412 0.4446 0.2642 0.066 Uiso 1 1 calc R . . H1B H 0.0591 0.3519 0.2568 0.066 Uiso 1 1 calc R . . C3 C 0.2183(7) 0.5492(6) 0.1021(3) 0.0513(13) Uani 1 1 d . . . C4 C 0.2413(7) 0.4937(6) -0.0233(3) 0.0537(14) Uani 1 1 d . . . C9 C 0.1561(8) 0.4112(7) -0.0819(3) 0.0690(17) Uani 1 1 d . . . H9 H 0.0573 0.3503 -0.0784 0.083 Uiso 1 1 calc R . . C7 C 0.3637(9) 0.5116(7) -0.1506(3) 0.0639(17) Uani 1 1 d . . . C5 C 0.3902(9) 0.5864(8) -0.0309(3) 0.081(2) Uani 1 1 d . . . H5 H 0.4501 0.6429 0.0071 0.097 Uiso 1 1 calc R . . C8 C 0.2169(9) 0.4189(8) -0.1451(3) 0.0716(18) Uani 1 1 d . . . H8 H 0.1599 0.3625 -0.1837 0.086 Uiso 1 1 calc R . . C6 C 0.4469(10) 0.5926(9) -0.0958(4) 0.084(2) Uani 1 1 d . . . H6 H 0.5445 0.6543 -0.1008 0.100 Uiso 1 1 calc R . . N3 N 0.1748(6) 0.4732(5) 0.0384(2) 0.0650(15) Uani 1 1 d . . . H3 H 0.0930 0.4014 0.0368 0.078 Uiso 1 1 calc R . . N2 N 0.1339(6) 0.4827(5) 0.1517(2) 0.0573(12) Uani 1 1 d . . . H2 H 0.0626 0.4038 0.1406 0.069 Uiso 1 1 calc R . . N4 N 0.4292(10) 0.5191(8) -0.2177(3) 0.081(2) Uani 1 1 d . . . O2 O 0.3534(9) 0.4423(7) -0.2670(3) 0.110(2) Uani 1 1 d . . . O1 O 0.5583(8) 0.6077(8) -0.2202(3) 0.109(2) Uani 1 1 d . . . C13 C 0.6457(6) 0.9185(6) 0.3587(3) 0.0469(12) Uani 1 1 d . . . C10 C 0.2462(7) 0.4357(6) 0.3577(3) 0.0543(14) Uani 1 1 d . . . H10A H 0.2986 0.4301 0.3166 0.065 Uiso 1 1 calc R . . H10B H 0.1987 0.3428 0.3699 0.065 Uiso 1 1 calc R . . C14 C 0.7887(6) 1.0255(6) 0.3712(3) 0.0518(13) Uani 1 1 d . . . H14 H 0.8187 1.0747 0.4146 0.062 Uiso 1 1 calc R . . C18 C 0.6011(7) 0.8488(6) 0.2940(3) 0.0552(14) Uani 1 1 d . . . H18 H 0.5041 0.7813 0.2851 0.066 Uiso 1 1 calc R . . C16 C 0.8408(7) 0.9816(6) 0.2556(3) 0.0587(15) Uani 1 1 d . . . C11 C 0.3641(7) 0.5188(6) 0.4156(3) 0.0566(14) Uani 1 1 d . . . H11A H 0.3124 0.5265 0.4567 0.068 Uiso 1 1 calc R . . H11B H 0.4326 0.4702 0.4258 0.068 Uiso 1 1 calc R . . C15 C 0.8845(7) 1.0573(6) 0.3189(3) 0.0539(13) Uani 1 1 d . . . H15 H 0.9783 1.1297 0.3265 0.065 Uiso 1 1 calc R . . C17 C 0.6970(7) 0.8773(6) 0.2425(3) 0.0593(15) Uani 1 1 d . . . H17 H 0.6669 0.8277 0.1991 0.071 Uiso 1 1 calc R . . C12 C 0.4538(6) 0.7732(6) 0.4317(3) 0.0479(12) Uani 1 1 d . . . N6 N 0.5512(5) 0.8948(5) 0.4132(3) 0.0526(11) Uani 1 1 d . . . H6A H 0.5551 0.9673 0.4387 0.063 Uiso 1 1 calc R . . N5 N 0.4541(6) 0.6566(5) 0.3993(3) 0.0588(13) Uani 1 1 d . . . H5A H 0.5119 0.6627 0.3660 0.071 Uiso 1 1 calc R . . N7 N 0.9427(7) 1.0103(6) 0.2005(3) 0.0709(15) Uani 1 1 d . . . O3 O 1.0550(7) 1.1136(6) 0.2080(3) 0.0883(16) Uani 1 1 d . . . O4 O 0.9158(9) 0.9265(7) 0.1505(3) 0.118(2) Uani 1 1 d . . . C22 C 0.1953(6) 0.9663(6) 0.3680(3) 0.0460(12) Uani 1 1 d . . . C21 C -0.0080(6) 0.7933(5) 0.4251(3) 0.0428(11) Uani 1 1 d . . . C19 C 0.0094(7) 0.4556(6) 0.3912(3) 0.0518(13) Uani 1 1 d . . . H19A H 0.0604 0.4690 0.4372 0.062 Uiso 1 1 calc R . . H19B H -0.0551 0.3593 0.3818 0.062 Uiso 1 1 calc R . . C25 C 0.4075(7) 1.0724(6) 0.2748(3) 0.0533(14) Uani 1 1 d . . . C27 C 0.3213(6) 1.0871(6) 0.3862(3) 0.0501(13) Uani 1 1 d . . . H27 H 0.3344 1.1322 0.4304 0.060 Uiso 1 1 calc R . . C20 C -0.0891(6) 0.5419(5) 0.3893(3) 0.0504(13) Uani 1 1 d . . . H20A H -0.1594 0.5126 0.3480 0.060 Uiso 1 1 calc R . . H20B H -0.1489 0.5299 0.4290 0.060 Uiso 1 1 calc R . . C26 C 0.4272(7) 1.1409(6) 0.3393(3) 0.0524(13) Uani 1 1 d . . . H26 H 0.5103 1.2222 0.3516 0.063 Uiso 1 1 calc R . . C23 C 0.1767(7) 0.9009(6) 0.3010(3) 0.0515(13) Uani 1 1 d . . . H23 H 0.0929 0.8208 0.2877 0.062 Uiso 1 1 calc R . . C24 C 0.2838(8) 0.9560(7) 0.2542(3) 0.0591(15) Uani 1 1 d . . . H24 H 0.2710 0.9138 0.2093 0.071 Uiso 1 1 calc R . . N9 N 0.0912(5) 0.9219(4) 0.4174(2) 0.0455(10) Uani 1 1 d . . . H9A H 0.0893 0.9857 0.4477 0.055 Uiso 1 1 calc R . . N8 N 0.0073(5) 0.6871(4) 0.3899(2) 0.0487(11) Uani 1 1 d . . . H8A H 0.0824 0.7047 0.3643 0.058 Uiso 1 1 calc R . . N10 N 0.5234(7) 1.1266(7) 0.2260(3) 0.0692(16) Uani 1 1 d . . . O6 O 0.4951(8) 1.0753(7) 0.1670(3) 0.1012(19) Uani 1 1 d . . . O5 O 0.6414(6) 1.2189(6) 0.2469(3) 0.0867(16) Uani 1 1 d . . . C28 C 0.8415(13) 0.0449(13) -0.0436(5) 0.119(4) Uani 1 1 d . . . H28A H 0.7721 0.0408 -0.0824 0.179 Uiso 1 1 calc R . . H28B H 0.8733 -0.0330 -0.0487 0.179 Uiso 1 1 calc R . . H28C H 0.9294 0.1281 -0.0413 0.179 Uiso 1 1 calc R . . C29 C 0.6380(12) -0.0800(11) 0.0259(6) 0.120(4) Uani 1 1 d . . . H29A H 0.6741 -0.1529 0.0347 0.180 Uiso 1 1 calc R . . H29B H 0.5707 -0.1063 -0.0157 0.180 Uiso 1 1 calc R . . H29C H 0.5836 -0.0625 0.0637 0.180 Uiso 1 1 calc R . . N11 N 0.7665(7) 0.0430(7) 0.0182(3) 0.0822(18) Uani 1 1 d . . . C30 C 0.8153(9) 0.1494(8) 0.0670(4) 0.082(2) Uani 1 1 d . . . H30 H 0.7630 0.1425 0.1065 0.099 Uiso 1 1 calc R . . O7 O 0.9219(7) 0.2535(6) 0.0635(3) 0.103(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S3 0.0591(9) 0.0513(9) 0.0571(8) 0.0090(6) 0.0268(7) 0.0201(7) S2 0.0551(9) 0.0583(10) 0.0537(8) -0.0042(7) 0.0114(6) 0.0070(7) S1 0.0948(14) 0.0559(10) 0.0561(9) -0.0090(7) 0.0279(9) -0.0166(9) N1 0.051(3) 0.039(2) 0.044(2) 0.0025(18) 0.0171(19) 0.008(2) C2 0.071(4) 0.047(3) 0.040(3) -0.001(2) 0.011(3) 0.001(3) C1 0.065(4) 0.044(3) 0.046(3) 0.005(2) 0.015(3) 0.007(3) C3 0.052(3) 0.046(3) 0.045(3) -0.004(2) 0.011(2) 0.005(3) C4 0.067(4) 0.050(3) 0.040(3) -0.003(2) 0.010(2) 0.016(3) C9 0.070(4) 0.062(4) 0.057(4) -0.005(3) 0.001(3) 0.003(3) C7 0.098(5) 0.060(4) 0.045(3) 0.008(3) 0.026(3) 0.040(4) C5 0.078(5) 0.082(5) 0.048(3) -0.010(3) 0.019(3) -0.012(4) C8 0.098(5) 0.072(4) 0.040(3) -0.003(3) 0.002(3) 0.026(4) C6 0.086(5) 0.087(5) 0.070(4) 0.007(4) 0.038(4) 0.017(4) N3 0.070(3) 0.054(3) 0.044(2) -0.009(2) 0.009(2) -0.009(3) N2 0.067(3) 0.047(3) 0.043(2) -0.002(2) 0.015(2) 0.003(2) N4 0.132(6) 0.092(5) 0.050(3) 0.021(3) 0.028(4) 0.071(5) O2 0.191(7) 0.117(5) 0.046(3) 0.008(3) 0.026(3) 0.084(5) O1 0.122(5) 0.131(6) 0.091(4) 0.035(4) 0.066(4) 0.054(5) C13 0.041(3) 0.042(3) 0.058(3) 0.003(2) 0.005(2) 0.015(2) C10 0.062(4) 0.045(3) 0.060(3) 0.010(3) 0.021(3) 0.021(3) C14 0.045(3) 0.039(3) 0.064(3) 0.003(2) 0.002(3) 0.007(2) C18 0.044(3) 0.048(3) 0.066(4) 0.000(3) 0.007(3) 0.008(3) C16 0.059(4) 0.050(3) 0.073(4) 0.007(3) 0.016(3) 0.026(3) C11 0.055(3) 0.046(3) 0.069(4) 0.019(3) 0.008(3) 0.015(3) C15 0.047(3) 0.044(3) 0.066(3) 0.004(3) 0.000(3) 0.012(3) C17 0.067(4) 0.052(3) 0.055(3) -0.002(3) 0.006(3) 0.018(3) C12 0.040(3) 0.044(3) 0.053(3) 0.000(2) -0.001(2) 0.008(2) N6 0.044(3) 0.044(3) 0.062(3) -0.001(2) 0.013(2) 0.007(2) N5 0.058(3) 0.045(3) 0.071(3) 0.008(2) 0.023(2) 0.013(2) N7 0.080(4) 0.063(4) 0.073(4) 0.013(3) 0.025(3) 0.025(3) O3 0.086(4) 0.071(3) 0.103(4) 0.017(3) 0.046(3) 0.014(3) O4 0.139(6) 0.093(4) 0.093(4) -0.012(3) 0.055(4) 0.007(4) C22 0.049(3) 0.047(3) 0.048(3) 0.009(2) 0.017(2) 0.021(3) C21 0.045(3) 0.045(3) 0.043(2) 0.004(2) 0.009(2) 0.021(2) C19 0.061(3) 0.041(3) 0.051(3) 0.008(2) 0.023(3) 0.012(3) C25 0.052(3) 0.053(3) 0.065(3) 0.026(3) 0.024(3) 0.025(3) C27 0.049(3) 0.049(3) 0.051(3) 0.003(2) 0.012(2) 0.016(3) C20 0.049(3) 0.043(3) 0.053(3) 0.005(2) 0.016(2) 0.008(2) C26 0.051(3) 0.047(3) 0.057(3) 0.011(2) 0.014(2) 0.011(3) C23 0.057(3) 0.047(3) 0.047(3) 0.006(2) 0.010(2) 0.013(3) C24 0.077(4) 0.056(4) 0.048(3) 0.008(3) 0.020(3) 0.027(3) N9 0.050(3) 0.043(2) 0.045(2) 0.0036(18) 0.0174(19) 0.017(2) N8 0.045(2) 0.041(2) 0.059(3) 0.002(2) 0.020(2) 0.012(2) N10 0.076(4) 0.069(4) 0.075(4) 0.028(3) 0.037(3) 0.032(3) O6 0.134(5) 0.102(4) 0.064(3) 0.014(3) 0.052(3) 0.031(4) O5 0.067(3) 0.090(4) 0.094(4) 0.031(3) 0.031(3) 0.009(3) C28 0.122(8) 0.156(11) 0.069(5) 0.004(6) 0.020(5) 0.037(8) C29 0.109(7) 0.087(6) 0.116(7) -0.008(5) 0.032(6) -0.024(5) N11 0.079(4) 0.069(4) 0.073(4) 0.006(3) 0.023(3) -0.008(3) C30 0.080(5) 0.068(5) 0.070(4) -0.002(4) 0.018(4) -0.008(4) O7 0.097(4) 0.071(4) 0.092(4) 0.005(3) 0.004(3) -0.028(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S3 C21 1.701(5) . ? S2 C12 1.695(6) . ? S1 C3 1.657(6) . ? N1 C1 1.459(7) . ? N1 C10 1.462(7) . ? N1 C19 1.473(6) . ? C2 N2 1.447(7) . ? C2 C1 1.515(8) . ? C3 N2 1.359(7) . ? C3 N3 1.379(7) . ? C4 N3 1.382(7) . ? C4 C9 1.396(8) . ? C4 C5 1.414(9) . ? C9 C8 1.382(9) . ? C7 C6 1.330(11) . ? C7 C8 1.390(11) . ? C7 N4 1.472(8) . ? C5 C6 1.398(9) . ? N4 O2 1.216(9) . ? N4 O1 1.243(10) . ? C13 C18 1.372(8) . ? C13 N6 1.401(7) . ? C13 C14 1.403(8) . ? C10 C11 1.513(8) . ? C14 C15 1.377(8) . ? C18 C17 1.365(8) . ? C16 C15 1.372(9) . ? C16 C17 1.398(9) . ? C16 N7 1.454(8) . ? C11 N5 1.460(7) . ? C12 N5 1.327(7) . ? C12 N6 1.367(7) . ? N7 O3 1.204(8) . ? N7 O4 1.210(8) . ? C22 C27 1.395(8) . ? C22 N9 1.396(6) . ? C22 C23 1.398(7) . ? C21 N8 1.311(6) . ? C21 N9 1.363(7) . ? C19 C20 1.501(8) . ? C25 C24 1.364(9) . ? C25 C26 1.368(8) . ? C25 N10 1.472(7) . ? C27 C26 1.387(7) . ? C20 N8 1.465(7) . ? C23 C24 1.396(8) . ? N10 O6 1.206(8) . ? N10 O5 1.206(8) . ? C28 N11 1.426(10) . ? C29 N11 1.442(10) . ? N11 C30 1.333(10) . ? C30 O7 1.199(9) . ? 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 C1 N1 C10 110.7(4) . . ? C1 N1 C19 113.8(5) . . ? C10 N1 C19 110.9(4) . . ? N2 C2 C1 111.8(5) . . ? N1 C1 C2 109.2(5) . . ? N2 C3 N3 111.7(5) . . ? N2 C3 S1 121.7(4) . . ? N3 C3 S1 126.6(4) . . ? N3 C4 C9 116.8(6) . . ? N3 C4 C5 125.2(5) . . ? C9 C4 C5 118.0(5) . . ? C8 C9 C4 120.8(7) . . ? C6 C7 C8 121.0(6) . . ? C6 C7 N4 119.3(7) . . ? C8 C7 N4 119.7(6) . . ? C6 C5 C4 119.6(6) . . ? C9 C8 C7 119.5(6) . . ? C7 C6 C5 121.1(7) . . ? C3 N3 C4 130.6(5) . . ? C3 N2 C2 121.3(5) . . ? O2 N4 O1 124.4(7) . . ? O2 N4 C7 118.7(8) . . ? O1 N4 C7 116.9(7) . . ? C18 C13 N6 123.3(5) . . ? C18 C13 C14 119.6(5) . . ? N6 C13 C14 117.0(5) . . ? N1 C10 C11 115.4(5) . . ? C15 C14 C13 119.8(6) . . ? C17 C18 C13 120.9(6) . . ? C15 C16 C17 120.7(6) . . ? C15 C16 N7 120.5(6) . . ? C17 C16 N7 118.8(6) . . ? N5 C11 C10 112.9(5) . . ? C16 C15 C14 119.6(6) . . ? C18 C17 C16 119.2(6) . . ? N5 C12 N6 118.4(5) . . ? N5 C12 S2 123.4(4) . . ? N6 C12 S2 118.1(4) . . ? C12 N6 C13 129.4(5) . . ? C12 N5 C11 125.2(5) . . ? O3 N7 O4 122.4(6) . . ? O3 N7 C16 118.6(6) . . ? O4 N7 C16 118.9(6) . . ? C27 C22 N9 117.3(5) . . ? C27 C22 C23 118.6(5) . . ? N9 C22 C23 124.0(5) . . ? N8 C21 N9 118.8(4) . . ? N8 C21 S3 123.1(4) . . ? N9 C21 S3 118.1(4) . . ? N1 C19 C20 112.6(4) . . ? C24 C25 C26 122.1(5) . . ? C24 C25 N10 119.1(6) . . ? C26 C25 N10 118.7(6) . . ? C26 C27 C22 121.0(5) . . ? N8 C20 C19 109.8(4) . . ? C25 C26 C27 118.8(6) . . ? C24 C23 C22 120.0(6) . . ? C25 C24 C23 119.4(6) . . ? C21 N9 C22 130.1(4) . . ? C21 N8 C20 127.3(4) . . ? O6 N10 O5 123.3(6) . . ? O6 N10 C25 117.8(7) . . ? O5 N10 C25 118.9(6) . . ? C30 N11 C28 121.2(7) . . ? C30 N11 C29 121.9(7) . . ? C28 N11 C29 116.9(8) . . ? O7 C30 N11 124.6(7) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.673 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.134 data_Thiourea-F _database_code_depnum_ccdc_archive 'CCDC 796388' #TrackingRef 'CCDC 796388.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H69 F N12 O6 S3' _chemical_formula_weight 989.33 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' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0874(4) _cell_length_b 13.1320(4) _cell_length_c 35.7500(11) _cell_angle_alpha 79.965(2) _cell_angle_beta 86.542(3) _cell_angle_gamma 60.285(2) _cell_volume 5252.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9440 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.49 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 0.201 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.916 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and onega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49038 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0831 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 28.36 _reflns_number_total 25528 _reflns_number_gt 21878 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+0.0010P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21528 _refine_ls_number_parameters 1207 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1979 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.2466 _refine_ls_wR_factor_gt 0.2076 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 1.28986(11) 0.00759(12) 0.84622(3) 0.0712(4) Uani 1 1 d . . . S4 S 0.58719(13) 1.15297(11) 0.65577(4) 0.0763(4) Uani 1 1 d . . . S5 S 0.91642(12) 0.41530(11) 0.65312(4) 0.0773(4) Uani 1 1 d . . . S3 S 0.55529(13) 0.42414(12) 0.84122(4) 0.0857(5) Uani 1 1 d . . . S2 S 0.88067(14) -0.31996(12) 0.84534(4) 0.0850(4) Uani 1 1 d . . . S6 S 0.17573(12) 0.82917(14) 0.65829(4) 0.0875(5) Uani 1 1 d . . . F1 F 0.9031(2) 0.0556(2) 0.80823(6) 0.0583(6) Uani 1 1 d . . . N1 N 0.9081(3) 0.0070(3) 0.90700(9) 0.0609(10) Uani 1 1 d . . . C4 C 1.1569(4) 0.0618(3) 0.76251(11) 0.0484(10) Uani 1 1 d . . . C9 C 1.2532(4) 0.0785(4) 0.75355(12) 0.0614(12) Uani 1 1 d . . . H9 H 1.3016 0.0721 0.7729 0.074 Uiso 1 1 calc R . . C5 C 1.0861(4) 0.0722(4) 0.73215(12) 0.0591(12) Uani 1 1 d . . . H5 H 1.0212 0.0617 0.7376 0.071 Uiso 1 1 calc R . . C6 C 1.1102(4) 0.0970(4) 0.69518(12) 0.0620(12) Uani 1 1 d . . . H6 H 1.0629 0.1027 0.6757 0.074 Uiso 1 1 calc R . . C7 C 1.2054(4) 0.1135(4) 0.68718(12) 0.0575(12) Uani 1 1 d . . . C3 C 1.1651(4) 0.0144(4) 0.83385(12) 0.0516(11) Uani 1 1 d . . . C2 C 1.1142(4) -0.0268(5) 0.90065(11) 0.0696(13) Uani 1 1 d . . . H2A H 1.0984 0.0468 0.9084 0.084 Uiso 1 1 calc R . . H2B H 1.1951 -0.0863 0.9079 0.084 Uiso 1 1 calc R . . C8 C 1.2767(4) 0.1046(4) 0.71602(14) 0.0678(13) Uani 1 1 d . . . H8 H 1.3408 0.1161 0.7101 0.081 Uiso 1 1 calc R . . C1 C 1.0319(4) -0.0677(5) 0.92030(12) 0.0729(14) Uani 1 1 d . . . H1A H 1.0590 -0.1485 0.9165 0.087 Uiso 1 1 calc R . . H1B H 1.0363 -0.0692 0.9474 0.087 Uiso 1 1 calc R . . N3 N 1.1194(3) 0.0386(3) 0.79856(9) 0.0511(9) Uani 1 1 d . . . H3 H 1.0531 0.0399 0.7983 0.061 Uiso 1 1 calc R . . N2 N 1.0972(3) -0.0086(3) 0.86010(9) 0.0622(10) Uani 1 1 d . . . H2 H 1.0391 -0.0128 0.8519 0.075 Uiso 1 1 calc R . . N4 N 1.2321(4) 0.1390(4) 0.64797(13) 0.0743(12) Uani 1 1 d . . . O1 O 1.1671(4) 0.1494(4) 0.62312(11) 0.1004(13) Uani 1 1 d . . . O2 O 1.3201(4) 0.1480(4) 0.64101(10) 0.1044(13) Uani 1 1 d . . . C13 C 0.8853(4) -0.1597(4) 0.76180(14) 0.0573(11) Uani 1 1 d . . . C14 C 0.8785(4) -0.0713(4) 0.73252(14) 0.0653(13) Uani 1 1 d . . . H14 H 0.8721 -0.0022 0.7384 0.078 Uiso 1 1 calc R . . C12 C 0.8776(4) -0.1900(4) 0.83401(14) 0.0608(12) Uani 1 1 d . . . C11 C 0.8697(5) -0.1580(5) 0.90038(13) 0.0763(15) Uani 1 1 d . . . H11A H 0.9477 -0.2224 0.9088 0.092 Uiso 1 1 calc R . . H11B H 0.8139 -0.1859 0.9071 0.092 Uiso 1 1 calc R . . C15 C 0.8809(4) -0.0839(4) 0.69485(14) 0.0662(13) Uani 1 1 d . . . H15 H 0.8766 -0.0242 0.6756 0.079 Uiso 1 1 calc R . . C18 C 0.8956(4) -0.2626(4) 0.75179(15) 0.0718(14) Uani 1 1 d . . . H18 H 0.9011 -0.3237 0.7707 0.086 Uiso 1 1 calc R . . C16 C 0.8898(4) -0.1862(5) 0.68629(15) 0.0652(13) Uani 1 1 d . . . C17 C 0.8976(4) -0.2741(5) 0.71464(17) 0.0757(14) Uani 1 1 d . . . H17 H 0.9044 -0.3431 0.7085 0.091 Uiso 1 1 calc R . . C10 C 0.8391(5) -0.0529(5) 0.91960(13) 0.0769(15) Uani 1 1 d . . . H10A H 0.7562 0.0043 0.9148 0.092 Uiso 1 1 calc R . . H10B H 0.8514 -0.0799 0.9468 0.092 Uiso 1 1 calc R . . N6 N 0.8831(3) -0.1354(3) 0.79828(11) 0.0608(10) Uani 1 1 d . . . H6A H 0.8858 -0.0714 0.7984 0.073 Uiso 1 1 calc R . . N5 N 0.8665(3) -0.1228(4) 0.85977(11) 0.0704(11) Uani 1 1 d . . . H5A H 0.8566 -0.0529 0.8514 0.085 Uiso 1 1 calc R . . N7 N 0.8900(4) -0.1999(6) 0.64713(15) 0.0848(14) Uani 1 1 d . . . O3 O 0.8816(4) -0.1171(5) 0.62243(13) 0.1124(15) Uani 1 1 d . . . O4 O 0.8967(4) -0.2900(4) 0.63991(12) 0.1145(15) Uani 1 1 d . . . C21 C 0.6756(4) 0.3048(4) 0.83049(12) 0.0574(11) Uani 1 1 d . . . C20 C 0.7402(4) 0.2173(5) 0.89732(13) 0.0775(15) Uani 1 1 d . . . H20A H 0.6787 0.1979 0.9050 0.093 Uiso 1 1 calc R . . H20B H 0.7168 0.2946 0.9037 0.093 Uiso 1 1 calc R . . C19 C 0.8556(5) 0.1237(5) 0.91856(13) 0.0758(14) Uani 1 1 d . . . H19A H 0.9117 0.1521 0.9146 0.091 Uiso 1 1 calc R . . H19B H 0.8411 0.1150 0.9456 0.091 Uiso 1 1 calc R . . C22 C 0.6599(4) 0.3369(4) 0.75842(12) 0.0541(11) Uani 1 1 d . . . C25 C 0.5844(4) 0.4285(4) 0.68332(13) 0.0595(12) Uani 1 1 d . . . C27 C 0.7287(4) 0.2827(4) 0.72884(13) 0.0629(12) Uani 1 1 d . . . H27 H 0.8015 0.2146 0.7345 0.075 Uiso 1 1 calc R . . C26 C 0.6907(4) 0.3281(4) 0.69166(13) 0.0689(13) Uani 1 1 d . . . H26 H 0.7372 0.2906 0.6723 0.083 Uiso 1 1 calc R . . C24 C 0.5156(4) 0.4829(4) 0.71197(15) 0.0731(14) Uani 1 1 d . . . H24 H 0.4429 0.5511 0.7061 0.088 Uiso 1 1 calc R . . C23 C 0.5531(4) 0.4376(4) 0.74902(14) 0.0686(13) Uani 1 1 d . . . H23 H 0.5056 0.4756 0.7682 0.082 Uiso 1 1 calc R . . N9 N 0.7097(3) 0.2784(3) 0.79494(10) 0.0587(9) Uani 1 1 d . . . H9A H 0.7746 0.2127 0.7949 0.070 Uiso 1 1 calc R . . N8 N 0.7544(3) 0.2216(3) 0.85685(10) 0.0676(11) Uani 1 1 d . . . H8A H 0.8182 0.1665 0.8491 0.081 Uiso 1 1 calc R . . N10 N 0.5457(4) 0.4751(4) 0.64396(13) 0.0756(12) Uani 1 1 d . . . O5 O 0.4522(4) 0.5708(4) 0.63676(10) 0.1023(12) Uani 1 1 d . . . O6 O 0.6071(4) 0.4210(4) 0.61912(11) 0.1020(13) Uani 1 1 d . . . N11 N 0.5541(3) 0.8305(3) 0.59321(9) 0.0612(10) Uani 1 1 d . . . C31 C 0.5820(3) 0.9967(4) 0.73990(12) 0.0502(10) Uani 1 1 d . . . C36 C 0.5898(4) 0.9090(4) 0.76934(13) 0.0604(12) Uani 1 1 d . . . H36 H 0.6005 0.8376 0.7639 0.072 Uiso 1 1 calc R . . C30 C 0.5897(4) 1.0232(4) 0.66789(13) 0.0559(11) Uani 1 1 d . . . C34 C 0.5703(4) 1.0306(4) 0.81450(13) 0.0557(11) Uani 1 1 d . . . C29 C 0.5914(5) 0.9951(4) 0.60087(12) 0.0722(14) Uani 1 1 d . . . H29A H 0.6462 1.0242 0.5939 0.087 Uiso 1 1 calc R . . H29B H 0.5127 1.0595 0.5931 0.087 Uiso 1 1 calc R . . C32 C 0.5698(4) 1.1006(4) 0.74830(13) 0.0636(12) Uani 1 1 d . . . H32 H 0.5655 1.1597 0.7288 0.076 Uiso 1 1 calc R . . C35 C 0.5817(4) 0.9266(4) 0.80683(14) 0.0665(13) Uani 1 1 d . . . H35 H 0.5839 0.8688 0.8265 0.080 Uiso 1 1 calc R . . C33 C 0.5640(4) 1.1176(4) 0.78561(14) 0.0690(13) Uani 1 1 d . . . H33 H 0.5557 1.1879 0.7911 0.083 Uiso 1 1 calc R . . C28 C 0.6211(5) 0.8919(4) 0.58061(12) 0.0703(13) Uani 1 1 d . . . H28A H 0.6065 0.9213 0.5535 0.084 Uiso 1 1 calc R . . H28B H 0.7044 0.8351 0.5846 0.084 Uiso 1 1 calc R . . N13 N 0.5867(3) 0.9687(3) 0.70346(10) 0.0540(9) Uani 1 1 d . . . H13 H 0.5878 0.9025 0.7038 0.065 Uiso 1 1 calc R . . N12 N 0.5976(3) 0.9576(3) 0.64187(10) 0.0629(10) Uani 1 1 d . . . H12 H 0.6071 0.8878 0.6500 0.075 Uiso 1 1 calc R . . N14 N 0.5638(4) 1.0494(5) 0.85295(13) 0.0726(11) Uani 1 1 d . . . O8 O 0.5636(4) 0.9728(4) 0.87830(11) 0.1000(12) Uani 1 1 d . . . O7 O 0.5601(4) 1.1383(4) 0.86033(10) 0.1028(13) Uani 1 1 d . . . C40 C 0.8101(4) 0.4991(4) 0.73665(12) 0.0533(11) Uani 1 1 d . . . C41 C 0.7398(4) 0.5529(4) 0.76617(12) 0.0616(12) Uani 1 1 d . . . H41 H 0.6671 0.6209 0.7602 0.074 Uiso 1 1 calc R . . C39 C 0.7939(4) 0.5313(4) 0.66482(13) 0.0566(11) Uani 1 1 d . . . C42 C 0.7747(4) 0.5088(4) 0.80325(13) 0.0633(12) Uani 1 1 d . . . H42 H 0.7267 0.5459 0.8225 0.076 Uiso 1 1 calc R . . C45 C 0.9175(4) 0.3981(4) 0.74607(13) 0.0634(12) Uani 1 1 d . . . H45 H 0.9656 0.3604 0.7270 0.076 Uiso 1 1 calc R . . C43 C 0.8837(4) 0.4070(4) 0.81194(13) 0.0608(12) Uani 1 1 d . . . C38 C 0.7223(5) 0.6224(4) 0.59831(12) 0.0754(14) Uani 1 1 d . . . H38A H 0.7448 0.5464 0.5910 0.091 Uiso 1 1 calc R . . H38B H 0.7828 0.6431 0.5904 0.091 Uiso 1 1 calc R . . C44 C 0.9537(4) 0.3533(4) 0.78318(14) 0.0731(14) Uani 1 1 d . . . H44 H 1.0267 0.2856 0.7891 0.088 Uiso 1 1 calc R . . C37 C 0.6048(4) 0.7174(4) 0.57927(12) 0.0733(14) Uani 1 1 d . . . H37A H 0.6152 0.7313 0.5521 0.088 Uiso 1 1 calc R . . H37B H 0.5495 0.6879 0.5832 0.088 Uiso 1 1 calc R . . N16 N 0.7622(3) 0.5564(3) 0.70049(9) 0.0573(9) Uani 1 1 d . . . H16 H 0.6981 0.6228 0.7006 0.069 Uiso 1 1 calc R . . N15 N 0.7109(3) 0.6141(3) 0.63888(10) 0.0636(10) Uani 1 1 d . . . H15A H 0.6462 0.6660 0.6472 0.076 Uiso 1 1 calc R . . N17 N 0.9200(4) 0.3584(4) 0.85134(13) 0.0768(12) Uani 1 1 d . . . O10 O 1.0136(4) 0.2662(4) 0.85888(10) 0.1078(13) Uani 1 1 d . . . O9 O 0.8573(4) 0.4112(4) 0.87626(10) 0.1015(13) Uani 1 1 d . . . C49 C 0.3146(4) 0.7712(3) 0.74127(13) 0.0545(11) Uani 1 1 d . . . C50 C 0.3859(4) 0.7620(4) 0.77071(14) 0.0649(12) Uani 1 1 d . . . H50 H 0.4511 0.7716 0.7646 0.078 Uiso 1 1 calc R . . C48 C 0.3024(4) 0.8214(4) 0.66921(15) 0.0645(13) Uani 1 1 d . . . C51 C 0.3629(4) 0.7393(4) 0.80820(14) 0.0693(13) Uani 1 1 d . . . H51 H 0.4111 0.7342 0.8273 0.083 Uiso 1 1 calc R . . C54 C 0.2179(4) 0.7573(4) 0.75078(15) 0.0694(13) Uani 1 1 d . . . H54 H 0.1683 0.7644 0.7317 0.083 Uiso 1 1 calc R . . C52 C 0.2674(5) 0.7243(4) 0.81681(15) 0.0657(13) Uani 1 1 d . . . C47 C 0.3481(5) 0.8639(5) 0.60194(13) 0.0778(15) Uani 1 1 d . . . H47A H 0.2667 0.9234 0.5955 0.093 Uiso 1 1 calc R . . H47B H 0.3630 0.7909 0.5939 0.093 Uiso 1 1 calc R . . C53 C 0.1947(5) 0.7329(4) 0.78818(17) 0.0795(15) Uani 1 1 d . . . H53 H 0.1303 0.7221 0.7944 0.095 Uiso 1 1 calc R . . C46 C 0.4288(4) 0.9060(4) 0.58157(13) 0.0753(15) Uani 1 1 d . . . H46A H 0.4210 0.9101 0.5545 0.090 Uiso 1 1 calc R . . H46B H 0.4028 0.9860 0.5861 0.090 Uiso 1 1 calc R . . N19 N 0.3518(3) 0.7933(3) 0.70509(11) 0.0612(10) Uani 1 1 d . . . H19 H 0.4198 0.7885 0.7051 0.073 Uiso 1 1 calc R . . N18 N 0.3689(3) 0.8431(3) 0.64288(11) 0.0678(10) Uani 1 1 d . . . H18A H 0.4287 0.8451 0.6507 0.081 Uiso 1 1 calc R . . N20 N 0.2390(5) 0.7023(4) 0.85581(15) 0.0847(14) Uani 1 1 d . . . O12 O 0.1514(4) 0.6919(4) 0.86355(12) 0.1154(15) Uani 1 1 d . . . O11 O 0.3033(4) 0.6973(4) 0.88061(13) 0.1175(15) Uani 1 1 d . . . C56 C 0.8483(6) 0.2861(7) 0.56545(19) 0.111(2) Uani 1 1 d . . . C55 C 0.8797(6) 0.2003(6) 0.59976(17) 0.120(2) Uani 1 1 d . . . H55A H 0.8383 0.1570 0.6002 0.179 Uiso 1 1 calc R . . H55B H 0.8590 0.2406 0.6213 0.179 Uiso 1 1 calc R . . H55C H 0.9630 0.1462 0.6007 0.179 Uiso 1 1 calc R . . N21 N 0.8231(7) 0.3497(7) 0.53896(17) 0.158(3) Uani 1 1 d . . . C57 C 0.3867(7) 0.3178(6) 0.10079(17) 0.122(2) Uani 1 1 d . . . H57A H 0.3365 0.3141 0.1211 0.183 Uiso 1 1 calc R . . H57B H 0.3850 0.3927 0.0976 0.183 Uiso 1 1 calc R . . H57C H 0.4658 0.2543 0.1068 0.183 Uiso 1 1 calc R . . C58 C 0.3465(6) 0.3063(6) 0.0668(2) 0.105(2) Uani 1 1 d . . . N22 N 0.3110(6) 0.2971(6) 0.03989(17) 0.150(3) Uani 1 1 d . . . N23 N 0.2400(4) 0.4794(4) 0.57282(11) 0.0734(12) Uani 1 1 d . . . C60 C 0.1562(6) 0.7043(5) 0.56534(16) 0.125(2) Uani 1 1 d D . . H60A H 0.2307 0.6948 0.5556 0.149 Uiso 1 1 calc R . . H60B H 0.1574 0.7045 0.5924 0.149 Uiso 1 1 calc R . . C59 C 0.1449(6) 0.6003(5) 0.55918(17) 0.128(3) Uani 1 1 d D . . H59A H 0.0732 0.6082 0.5710 0.153 Uiso 1 1 calc R . . H59B H 0.1340 0.6073 0.5321 0.153 Uiso 1 1 calc R . . C62 C 0.0568(8) 0.9353(6) 0.54948(19) 0.163(3) Uani 1 1 d D . . H62A H 0.0625 0.9397 0.5757 0.245 Uiso 1 1 calc R . . H62B H -0.0155 1.0017 0.5383 0.245 Uiso 1 1 calc R . . H62C H 0.1221 0.9371 0.5363 0.245 Uiso 1 1 calc R . . C61 C 0.0588(5) 0.8218(5) 0.54658(16) 0.123(3) Uani 1 1 d D . . H61A H 0.0577 0.8182 0.5198 0.148 Uiso 1 1 calc R . . H61B H -0.0146 0.8286 0.5565 0.148 Uiso 1 1 calc R . . C64 C 0.1778(8) 0.3885(8) 0.5260(2) 0.186(4) Uani 1 1 d D . . H64A H 0.2518 0.3622 0.5131 0.223 Uiso 1 1 calc R . . H64B H 0.1250 0.4697 0.5142 0.223 Uiso 1 1 calc R . . C63 C 0.2001(7) 0.3897(8) 0.5665(2) 0.143(3) Uani 1 1 d D . . H63A H 0.2600 0.3105 0.5776 0.172 Uiso 1 1 calc R . . H63B H 0.1285 0.4076 0.5802 0.172 Uiso 1 1 calc R . . C65 C 0.1270(8) 0.3133(8) 0.5187(3) 0.203(5) Uani 1 1 d D . . H65A H 0.0683 0.3206 0.5375 0.243 Uiso 1 1 calc R . . H65B H 0.0864 0.3462 0.4940 0.243 Uiso 1 1 calc R . . C67 C 0.3450(6) 0.4598(5) 0.5489(2) 0.127(2) Uani 1 1 d D . . H67A H 0.3165 0.4920 0.5228 0.152 Uiso 1 1 calc R . . H67B H 0.3755 0.5076 0.5563 0.152 Uiso 1 1 calc R . . C69 C 0.5498(6) 0.3266(6) 0.5264(2) 0.155(3) Uani 1 1 d D . . H69A H 0.5200 0.3743 0.5015 0.186 Uiso 1 1 calc R . . H69B H 0.5869 0.3615 0.5383 0.186 Uiso 1 1 calc R . . C68 C 0.4468(5) 0.3367(6) 0.54953(18) 0.124(2) Uani 1 1 d D . . H68A H 0.4186 0.2891 0.5406 0.149 Uiso 1 1 calc R . . H68B H 0.4743 0.3021 0.5757 0.149 Uiso 1 1 calc R . . C71 C 0.2734(7) 0.4573(7) 0.61307(19) 0.156(3) Uani 1 1 d D . . H71A H 0.3192 0.4962 0.6146 0.188 Uiso 1 1 calc R . . H71B H 0.3273 0.3725 0.6195 0.188 Uiso 1 1 calc R . . C72 C 0.1882(7) 0.4895(9) 0.6447(2) 0.220(6) Uani 1 1 d D . . H72A H 0.1540 0.4382 0.6461 0.264 Uiso 1 1 calc R . . H72B H 0.1255 0.5694 0.6355 0.264 Uiso 1 1 calc R . . C73 C 0.2122(10) 0.4896(11) 0.6852(2) 0.280(8) Uani 1 1 d D . . H73A H 0.2570 0.5296 0.6869 0.335 Uiso 1 1 calc R . . H73B H 0.1400 0.5264 0.6989 0.335 Uiso 1 1 calc R . . N24 N 0.2420(4) 0.3016(4) 0.92841(11) 0.0722(11) Uani 1 1 d . . . C75 C 0.2630(5) 0.3935(6) 0.94139(15) 0.105(2) Uani 1 1 d D . . H75A H 0.2045 0.4712 0.9286 0.126 Uiso 1 1 calc R . . H75B H 0.2485 0.3910 0.9684 0.126 Uiso 1 1 calc R . . C77 C 0.3942(6) 0.4702(5) 0.95490(15) 0.101(2) Uani 1 1 d D . . H77A H 0.3306 0.5497 0.9458 0.122 Uiso 1 1 calc R . . H77B H 0.3845 0.4519 0.9819 0.122 Uiso 1 1 calc R . . C76 C 0.3816(5) 0.3837(6) 0.93516(15) 0.0980(19) Uani 1 1 d D . . H76A H 0.3924 0.4000 0.9081 0.118 Uiso 1 1 calc R . . H76B H 0.4423 0.3033 0.9449 0.118 Uiso 1 1 calc R . . C78 C 0.5083(6) 0.4711(8) 0.94960(18) 0.148(3) Uani 1 1 d D . . H78A H 0.5717 0.3954 0.9609 0.222 Uiso 1 1 calc R . . H78B H 0.5054 0.5324 0.9616 0.222 Uiso 1 1 calc R . . H78C H 0.5210 0.4860 0.9229 0.222 Uiso 1 1 calc R . . C79 C 0.3210(5) 0.1812(5) 0.95265(15) 0.0918(17) Uani 1 1 d . . . H79A H 0.4018 0.1564 0.9456 0.110 Uiso 1 1 calc R . . H79B H 0.3149 0.1925 0.9790 0.110 Uiso 1 1 calc R . . C80 C 0.2983(6) 0.0822(5) 0.95049(18) 0.1038(19) Uani 1 1 d . . . H80A H 0.3037 0.0698 0.9243 0.125 Uiso 1 1 calc R . . H80B H 0.2189 0.1041 0.9585 0.125 Uiso 1 1 calc R . . C81 C 0.3836(6) -0.0318(6) 0.9749(2) 0.131(2) Uani 1 1 d D . . H81A H 0.4622 -0.0554 0.9657 0.157 Uiso 1 1 calc R . . H81B H 0.3822 -0.0169 1.0006 0.157 Uiso 1 1 calc R . . C87 C 0.2676(6) 0.2928(5) 0.88734(15) 0.114(2) Uani 1 1 d D . . H87A H 0.2459 0.2371 0.8809 0.136 Uiso 1 1 calc R . . H87B H 0.3521 0.2574 0.8849 0.136 Uiso 1 1 calc R . . C83 C 0.1129(6) 0.3368(6) 0.9347(2) 0.121(2) Uani 1 1 d . . . H83A H 0.0646 0.4165 0.9209 0.145 Uiso 1 1 calc R . . H83B H 0.0965 0.2839 0.9236 0.145 Uiso 1 1 calc R . . C84 C 0.0747(7) 0.3343(7) 0.9759(2) 0.144(3) Uani 1 1 d D . . H84A H 0.1189 0.2532 0.9891 0.173 Uiso 1 1 calc R . . H84B H 0.0968 0.3823 0.9875 0.173 Uiso 1 1 calc R . . C88 C 0.2115(8) 0.4026(6) 0.85775(17) 0.174(4) Uani 1 1 d D . . H88A H 0.2207 0.4638 0.8663 0.209 Uiso 1 1 calc R . . H88B H 0.1278 0.4299 0.8566 0.209 Uiso 1 1 calc R . . C85 C -0.0536(7) 0.3773(10) 0.9822(3) 0.200(4) Uani 1 1 d D . . H85A H -0.0705 0.3943 1.0079 0.240 Uiso 1 1 calc R . . H85B H -0.0990 0.4514 0.9650 0.240 Uiso 1 1 calc R . . C82 C 0.3608(8) -0.1336(6) 0.9762(2) 0.166(3) Uani 1 1 d D . . H82A H 0.2858 -0.1140 0.9872 0.249 Uiso 1 1 calc R . . H82B H 0.4215 -0.2033 0.9914 0.249 Uiso 1 1 calc R . . H82C H 0.3604 -0.1486 0.9509 0.249 Uiso 1 1 calc R . . C70 C 0.6428(7) 0.2042(6) 0.5208(2) 0.182(4) Uani 1 1 d D . . H70A H 0.6939 0.1655 0.5430 0.274 Uiso 1 1 calc R . . H70B H 0.6878 0.2096 0.4991 0.274 Uiso 1 1 calc R . . H70C H 0.6062 0.1590 0.5168 0.274 Uiso 1 1 calc R . . F2 F 0.56750(19) 0.77777(19) 0.69170(6) 0.0582(6) Uani 1 1 d . . . C66 C 0.2107(10) 0.1834(9) 0.5192(3) 0.263(6) Uani 1 1 d D . . H66A H 0.2798 0.1736 0.5056 0.394 Uiso 1 1 calc R . . H66B H 0.1733 0.1498 0.5072 0.394 Uiso 1 1 calc R . . H66C H 0.2326 0.1437 0.5450 0.394 Uiso 1 1 calc R . . C86 C -0.0945(11) 0.2925(10) 0.9767(4) 0.285(8) Uani 1 1 d D . . H86A H -0.0372 0.2132 0.9877 0.427 Uiso 1 1 calc R . . H86B H -0.1041 0.2959 0.9500 0.427 Uiso 1 1 calc R . . H86C H -0.1684 0.3141 0.9887 0.427 Uiso 1 1 calc R . . C89 C 0.2561(10) 0.3925(10) 0.81815(18) 0.259(7) Uani 1 1 d D . . H89A H 0.2510 0.4676 0.8068 0.310 Uiso 1 1 calc R . . H89B H 0.3387 0.3324 0.8199 0.310 Uiso 1 1 calc R . . C74 C 0.283(3) 0.3586(11) 0.6995(8) 0.61(2) Uiso 1 1 d D . . H74A H 0.3424 0.3438 0.7175 0.920 Uiso 1 1 calc R . . H74B H 0.3201 0.3178 0.6785 0.920 Uiso 1 1 calc R . . H74C H 0.2323 0.3302 0.7115 0.920 Uiso 1 1 calc R . . C90 C 0.194(3) 0.362(3) 0.7918(9) 0.69(3) Uiso 1 1 d D . . H90A H 0.1225 0.4318 0.7820 1.033 Uiso 1 1 calc R . . H90B H 0.1765 0.3028 0.8054 1.033 Uiso 1 1 calc R . . H90C H 0.2441 0.3308 0.7711 1.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0605(8) 0.0952(10) 0.0685(8) -0.0163(7) -0.0042(6) -0.0448(7) S4 0.0998(11) 0.0619(8) 0.0759(9) -0.0013(6) -0.0038(7) -0.0489(8) S5 0.0727(9) 0.0640(8) 0.0783(9) -0.0224(6) 0.0049(7) -0.0181(7) S3 0.0837(10) 0.0688(9) 0.0794(9) -0.0225(7) 0.0180(7) -0.0173(7) S2 0.0982(11) 0.0704(9) 0.0993(10) -0.0103(7) 0.0028(8) -0.0525(8) S6 0.0632(9) 0.1164(12) 0.0911(10) -0.0283(8) -0.0036(7) -0.0465(9) F1 0.0567(16) 0.0617(15) 0.0616(15) -0.0142(11) 0.0012(11) -0.0319(13) N1 0.068(3) 0.071(3) 0.049(2) -0.0104(18) 0.0051(18) -0.038(2) C4 0.047(3) 0.036(2) 0.054(3) -0.0056(18) -0.002(2) -0.015(2) C9 0.053(3) 0.072(3) 0.060(3) -0.001(2) -0.008(2) -0.034(3) C5 0.045(3) 0.072(3) 0.060(3) -0.012(2) 0.003(2) -0.028(2) C6 0.055(3) 0.070(3) 0.051(3) -0.007(2) -0.007(2) -0.024(3) C7 0.050(3) 0.051(3) 0.051(3) 0.000(2) 0.005(2) -0.013(2) C3 0.054(3) 0.052(3) 0.050(3) -0.0098(19) -0.004(2) -0.027(2) C2 0.078(4) 0.093(4) 0.047(3) -0.004(2) -0.010(2) -0.050(3) C8 0.050(3) 0.074(3) 0.074(4) -0.001(3) 0.008(3) -0.031(3) C1 0.079(4) 0.099(4) 0.046(3) -0.002(2) -0.007(2) -0.049(3) N3 0.042(2) 0.063(2) 0.051(2) -0.0078(17) -0.0002(16) -0.0282(18) N2 0.061(3) 0.088(3) 0.048(2) -0.0054(19) -0.0064(18) -0.046(2) N4 0.062(3) 0.070(3) 0.071(3) -0.003(2) 0.005(3) -0.021(2) O1 0.094(3) 0.125(3) 0.063(2) 0.003(2) -0.004(2) -0.045(3) O2 0.086(3) 0.137(4) 0.080(3) 0.005(2) 0.012(2) -0.055(3) C13 0.045(3) 0.060(3) 0.075(3) -0.021(2) 0.003(2) -0.029(2) C14 0.067(3) 0.066(3) 0.080(4) -0.024(3) 0.005(2) -0.042(3) C12 0.054(3) 0.063(3) 0.075(3) -0.016(3) 0.008(2) -0.036(2) C11 0.096(4) 0.093(4) 0.065(3) -0.007(3) 0.008(3) -0.068(3) C15 0.065(3) 0.073(3) 0.072(3) -0.013(3) 0.007(2) -0.042(3) C18 0.080(4) 0.067(3) 0.084(4) -0.013(3) 0.002(3) -0.048(3) C16 0.050(3) 0.085(4) 0.072(4) -0.031(3) 0.008(2) -0.037(3) C17 0.071(4) 0.075(4) 0.092(4) -0.038(3) 0.008(3) -0.038(3) C10 0.081(4) 0.099(4) 0.058(3) -0.014(3) 0.011(3) -0.051(3) N6 0.063(3) 0.056(2) 0.074(3) -0.017(2) 0.0048(19) -0.036(2) N5 0.088(3) 0.071(3) 0.067(3) -0.008(2) 0.007(2) -0.052(2) N7 0.061(3) 0.109(4) 0.093(4) -0.048(3) 0.012(2) -0.040(3) O3 0.129(4) 0.145(4) 0.091(3) -0.040(3) 0.026(3) -0.085(3) O4 0.129(4) 0.105(3) 0.117(3) -0.058(3) -0.005(3) -0.051(3) C21 0.064(3) 0.057(3) 0.052(3) -0.012(2) 0.004(2) -0.031(2) C20 0.078(4) 0.086(4) 0.061(3) -0.022(3) 0.009(3) -0.032(3) C19 0.095(4) 0.086(4) 0.051(3) -0.020(3) 0.004(3) -0.046(3) C22 0.057(3) 0.045(3) 0.069(3) -0.018(2) 0.004(2) -0.029(2) C25 0.065(3) 0.049(3) 0.066(3) -0.008(2) -0.005(2) -0.028(3) C27 0.065(3) 0.049(3) 0.062(3) -0.010(2) 0.005(2) -0.019(2) C26 0.083(4) 0.063(3) 0.065(3) -0.019(2) 0.009(3) -0.038(3) C24 0.066(3) 0.054(3) 0.086(4) -0.006(3) -0.008(3) -0.021(3) C23 0.065(3) 0.059(3) 0.073(3) -0.019(2) 0.006(3) -0.023(3) N9 0.058(2) 0.052(2) 0.061(2) -0.0136(18) 0.0035(18) -0.0218(18) N8 0.070(3) 0.068(3) 0.054(2) -0.0198(19) 0.0087(19) -0.024(2) N10 0.081(3) 0.067(3) 0.081(3) -0.005(2) -0.007(3) -0.040(3) O5 0.095(3) 0.089(3) 0.089(3) 0.006(2) -0.019(2) -0.024(2) O6 0.119(3) 0.093(3) 0.076(3) -0.019(2) 0.004(2) -0.037(3) N11 0.067(3) 0.063(2) 0.049(2) -0.0073(18) -0.0026(18) -0.029(2) C31 0.041(3) 0.052(3) 0.060(3) -0.007(2) -0.0001(19) -0.025(2) C36 0.070(3) 0.060(3) 0.063(3) -0.011(2) -0.001(2) -0.040(3) C30 0.051(3) 0.053(3) 0.058(3) -0.004(2) -0.001(2) -0.023(2) C34 0.048(3) 0.067(3) 0.057(3) -0.017(2) 0.006(2) -0.030(2) C29 0.088(4) 0.073(3) 0.054(3) 0.002(2) 0.002(2) -0.043(3) C32 0.073(3) 0.057(3) 0.063(3) -0.007(2) 0.004(2) -0.034(3) C35 0.063(3) 0.070(3) 0.070(3) -0.003(2) -0.004(2) -0.038(3) C33 0.071(4) 0.069(3) 0.077(4) -0.021(3) 0.009(3) -0.040(3) C28 0.087(4) 0.075(3) 0.054(3) -0.010(2) 0.008(2) -0.045(3) N13 0.058(2) 0.048(2) 0.063(2) -0.0107(17) 0.0033(17) -0.0302(18) N12 0.081(3) 0.053(2) 0.059(2) -0.0072(18) 0.0045(19) -0.038(2) N14 0.068(3) 0.089(3) 0.068(3) -0.013(3) 0.000(2) -0.044(3) O8 0.121(3) 0.128(3) 0.072(3) -0.024(2) 0.009(2) -0.076(3) O7 0.137(4) 0.103(3) 0.086(3) -0.033(2) 0.002(2) -0.066(3) C40 0.060(3) 0.046(2) 0.058(3) -0.011(2) -0.008(2) -0.028(2) C41 0.064(3) 0.048(3) 0.061(3) -0.004(2) -0.010(2) -0.019(2) C39 0.060(3) 0.051(3) 0.064(3) -0.016(2) 0.000(2) -0.029(2) C42 0.064(3) 0.054(3) 0.066(3) -0.017(2) -0.001(2) -0.023(2) C45 0.057(3) 0.053(3) 0.067(3) -0.017(2) -0.005(2) -0.014(2) C43 0.076(4) 0.051(3) 0.058(3) -0.004(2) -0.014(2) -0.033(3) C38 0.088(4) 0.067(3) 0.061(3) -0.015(2) 0.001(3) -0.028(3) C44 0.072(4) 0.051(3) 0.082(4) -0.007(3) -0.014(3) -0.019(3) C37 0.091(4) 0.078(3) 0.048(3) -0.018(2) -0.003(2) -0.037(3) N16 0.058(2) 0.045(2) 0.057(2) -0.0103(17) -0.0049(18) -0.0159(18) N15 0.062(3) 0.062(2) 0.054(2) -0.0159(18) -0.0011(18) -0.019(2) N17 0.096(4) 0.057(3) 0.079(3) -0.003(2) -0.026(3) -0.038(3) O10 0.118(3) 0.082(3) 0.094(3) 0.001(2) -0.039(2) -0.027(3) O9 0.128(4) 0.100(3) 0.061(2) -0.011(2) -0.014(2) -0.043(3) C49 0.043(3) 0.042(2) 0.068(3) -0.012(2) 0.002(2) -0.012(2) C50 0.049(3) 0.067(3) 0.076(4) -0.011(2) 0.004(2) -0.027(2) C48 0.053(3) 0.056(3) 0.081(4) -0.022(2) 0.002(3) -0.021(2) C51 0.058(3) 0.064(3) 0.076(4) -0.014(2) 0.001(3) -0.022(3) C54 0.053(3) 0.078(3) 0.080(4) -0.019(3) 0.004(3) -0.033(3) C52 0.060(4) 0.049(3) 0.075(4) -0.005(2) 0.011(3) -0.019(2) C47 0.073(4) 0.084(4) 0.075(4) -0.010(3) -0.015(3) -0.037(3) C53 0.063(4) 0.070(3) 0.100(4) -0.016(3) 0.020(3) -0.030(3) C46 0.079(4) 0.078(3) 0.055(3) 0.000(2) -0.007(3) -0.031(3) N19 0.045(2) 0.067(2) 0.070(3) -0.0131(19) -0.0055(19) -0.0246(19) N18 0.057(3) 0.085(3) 0.066(3) -0.010(2) -0.004(2) -0.039(2) N20 0.088(4) 0.063(3) 0.087(4) -0.004(2) 0.014(3) -0.029(3) O12 0.125(4) 0.124(4) 0.116(3) -0.022(3) 0.047(3) -0.079(3) O11 0.117(4) 0.133(4) 0.083(3) 0.013(3) -0.005(3) -0.056(3) C56 0.120(6) 0.145(7) 0.062(4) -0.031(4) 0.010(4) -0.058(5) C55 0.130(6) 0.126(6) 0.083(4) -0.027(4) 0.000(4) -0.045(5) N21 0.198(7) 0.203(7) 0.074(4) 0.008(4) -0.005(4) -0.110(6) C57 0.169(7) 0.150(6) 0.073(4) -0.019(4) 0.009(4) -0.098(6) C58 0.119(6) 0.114(5) 0.073(5) 0.010(4) 0.012(4) -0.059(4) N22 0.172(6) 0.192(7) 0.076(4) -0.007(4) -0.010(4) -0.086(5) N23 0.069(3) 0.086(3) 0.063(3) 0.013(2) -0.004(2) -0.043(3) C60 0.179(8) 0.111(5) 0.074(4) -0.002(4) -0.009(4) -0.067(5) C59 0.142(6) 0.104(5) 0.087(5) 0.009(4) -0.002(4) -0.030(5) C62 0.250(10) 0.112(6) 0.102(5) -0.029(4) -0.009(5) -0.065(6) C61 0.133(6) 0.107(5) 0.066(4) -0.005(3) -0.003(3) -0.015(5) C64 0.123(8) 0.180(9) 0.255(13) -0.049(9) -0.022(7) -0.068(7) C63 0.098(6) 0.186(9) 0.148(7) -0.018(6) 0.009(5) -0.074(6) C65 0.140(9) 0.145(9) 0.314(14) 0.035(9) -0.061(8) -0.079(8) C67 0.111(6) 0.103(6) 0.179(7) -0.023(5) -0.013(5) -0.061(5) C69 0.098(6) 0.128(7) 0.234(9) -0.013(6) 0.034(6) -0.059(5) C68 0.133(7) 0.126(6) 0.123(5) -0.024(4) -0.007(5) -0.069(6) C71 0.197(9) 0.121(6) 0.106(6) 0.037(5) -0.045(6) -0.057(6) C72 0.183(10) 0.209(11) 0.146(9) 0.017(7) 0.054(8) -0.024(8) C73 0.216(12) 0.40(2) 0.085(6) 0.070(9) -0.013(6) -0.081(12) N24 0.072(3) 0.074(3) 0.067(3) -0.024(2) -0.014(2) -0.028(2) C75 0.132(6) 0.109(5) 0.077(4) -0.026(3) -0.016(4) -0.057(4) C77 0.168(7) 0.106(5) 0.058(3) -0.016(3) 0.007(4) -0.089(5) C76 0.106(5) 0.128(5) 0.077(4) -0.029(4) 0.015(3) -0.067(4) C78 0.201(9) 0.223(9) 0.098(5) -0.047(5) 0.030(5) -0.160(8) C79 0.070(4) 0.103(5) 0.098(4) -0.033(3) -0.003(3) -0.033(4) C80 0.094(5) 0.089(4) 0.124(5) -0.021(4) -0.005(4) -0.040(4) C81 0.116(6) 0.101(5) 0.173(7) -0.008(5) -0.042(5) -0.052(5) C87 0.141(6) 0.128(6) 0.087(5) -0.039(4) -0.011(4) -0.069(5) C83 0.103(6) 0.089(5) 0.151(7) -0.017(4) -0.031(5) -0.030(4) C84 0.116(7) 0.160(7) 0.171(8) -0.068(6) 0.038(6) -0.070(6) C88 0.266(11) 0.123(6) 0.109(6) 0.004(5) -0.065(6) -0.076(7) C85 0.140(10) 0.184(11) 0.251(12) -0.059(9) -0.005(8) -0.052(8) C82 0.181(9) 0.107(6) 0.189(8) 0.028(5) -0.038(6) -0.068(6) C70 0.152(8) 0.170(9) 0.191(9) -0.035(7) 0.036(6) -0.055(7) F2 0.0555(15) 0.0538(14) 0.0610(15) -0.0085(11) -0.0014(11) -0.0238(12) C66 0.304(17) 0.206(13) 0.264(14) -0.025(11) 0.082(12) -0.127(13) C86 0.216(14) 0.312(18) 0.304(16) 0.085(13) -0.033(11) -0.151(14) C89 0.420(18) 0.238(12) 0.058(5) -0.015(6) -0.062(7) -0.113(12) _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 C3 1.673(4) . ? S4 C30 1.668(5) . ? S5 C39 1.669(4) . ? S3 C21 1.665(5) . ? S2 C12 1.665(5) . ? S6 C48 1.675(5) . ? N1 C19 1.460(6) . ? N1 C1 1.473(6) . ? N1 C10 1.473(6) . ? C4 N3 1.389(5) . ? C4 C9 1.393(6) . ? C4 C5 1.414(6) . ? C9 C8 1.381(6) . ? C5 C6 1.361(6) . ? C6 C7 1.373(6) . ? C7 C8 1.383(6) . ? C7 N4 1.447(6) . ? C3 N3 1.347(5) . ? C3 N2 1.353(5) . ? C2 N2 1.440(5) . ? C2 C1 1.514(6) . ? N4 O1 1.211(5) . ? N4 O2 1.220(5) . ? C13 N6 1.391(5) . ? C13 C14 1.392(6) . ? C13 C18 1.397(6) . ? C14 C15 1.382(6) . ? C12 N5 1.337(5) . ? C12 N6 1.368(5) . ? C11 N5 1.442(5) . ? C11 C10 1.511(6) . ? C15 C16 1.376(6) . ? C18 C17 1.360(6) . ? C16 C17 1.363(7) . ? C16 N7 1.442(6) . ? N7 O4 1.213(6) . ? N7 O3 1.239(6) . ? C21 N8 1.337(5) . ? C21 N9 1.366(5) . ? C20 N8 1.442(5) . ? C20 C19 1.530(7) . ? C22 C23 1.373(6) . ? C22 C27 1.395(6) . ? C22 N9 1.406(5) . ? C25 C26 1.363(6) . ? C25 C24 1.369(6) . ? C25 N10 1.446(6) . ? C27 C26 1.371(6) . ? C24 C23 1.365(6) . ? N10 O6 1.227(5) . ? N10 O5 1.243(5) . ? N11 C37 1.461(5) . ? N11 C28 1.466(5) . ? N11 C46 1.474(6) . ? C31 C32 1.378(6) . ? C31 C36 1.385(5) . ? C31 N13 1.404(5) . ? C36 C35 1.389(6) . ? C30 N12 1.341(5) . ? C30 N13 1.355(5) . ? C34 C33 1.372(6) . ? C34 C35 1.374(6) . ? C34 N14 1.429(6) . ? C29 N12 1.456(5) . ? C29 C28 1.516(6) . ? C32 C33 1.382(6) . ? N14 O7 1.218(5) . ? N14 O8 1.233(5) . ? C40 C45 1.379(6) . ? C40 N16 1.386(5) . ? C40 C41 1.399(6) . ? C41 C42 1.358(6) . ? C39 N15 1.349(5) . ? C39 N16 1.362(5) . ? C42 C43 1.392(6) . ? C45 C44 1.363(6) . ? C43 C44 1.375(6) . ? C43 N17 1.444(6) . ? C38 N15 1.440(5) . ? C38 C37 1.522(6) . ? N17 O10 1.223(5) . ? N17 O9 1.229(5) . ? C49 C54 1.380(6) . ? C49 N19 1.388(5) . ? C49 C50 1.398(6) . ? C50 C51 1.370(6) . ? C48 N18 1.334(6) . ? C48 N19 1.378(6) . ? C51 C52 1.368(7) . ? C54 C53 1.371(6) . ? C52 C53 1.392(7) . ? C52 N20 1.439(6) . ? C47 N18 1.458(6) . ? C47 C46 1.516(7) . ? N20 O12 1.230(6) . ? N20 O11 1.231(6) . ? C56 N21 1.092(8) . ? C56 C55 1.436(9) . ? C57 C58 1.414(9) . ? C58 N22 1.142(8) . ? N23 C71 1.466(7) . ? N23 C59 1.467(7) . ? N23 C67 1.506(7) . ? N23 C63 1.558(9) . ? C60 C59 1.4987(10) . ? C60 C61 1.4994(10) . ? C62 C61 1.4989(10) . ? C64 C63 1.4988(10) . ? C64 C65 1.4992(10) . ? C65 C66 1.4991(10) . ? C67 C68 1.4991(10) . ? C69 C70 1.4992(10) . ? C69 C68 1.4993(10) . ? C71 C72 1.4995(10) . ? C72 C73 1.5005(10) . ? C73 C74 1.5004(18) . ? N24 C87 1.497(6) . ? N24 C75 1.513(6) . ? N24 C79 1.526(6) . ? N24 C83 1.528(8) . ? C75 C76 1.4993(10) . ? C77 C78 1.4993(10) . ? C77 C76 1.514(7) . ? C79 C80 1.485(8) . ? C80 C81 1.501(8) . ? C81 C82 1.4997(10) . ? C87 C88 1.4993(10) . ? C83 C84 1.526(9) . ? C84 C85 1.4998(10) . ? C88 C89 1.5005(10) . ? C85 C86 1.4989(10) . ? C89 C90 1.502(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 N1 C1 111.2(4) . . ? C19 N1 C10 111.7(4) . . ? C1 N1 C10 111.5(4) . . ? N3 C4 C9 127.1(4) . . ? N3 C4 C5 115.0(4) . . ? C9 C4 C5 117.8(4) . . ? C8 C9 C4 120.0(4) . . ? C6 C5 C4 122.0(4) . . ? C5 C6 C7 119.0(4) . . ? C6 C7 C8 120.9(4) . . ? C6 C7 N4 119.3(5) . . ? C8 C7 N4 119.7(5) . . ? N3 C3 N2 110.8(4) . . ? N3 C3 S1 127.6(3) . . ? N2 C3 S1 121.6(3) . . ? N2 C2 C1 109.4(4) . . ? C7 C8 C9 120.2(4) . . ? N1 C1 C2 114.3(4) . . ? C3 N3 C4 133.5(4) . . ? C3 N2 C2 125.3(4) . . ? O1 N4 O2 122.2(5) . . ? O1 N4 C7 118.8(5) . . ? O2 N4 C7 119.0(5) . . ? N6 C13 C14 115.1(4) . . ? N6 C13 C18 127.2(5) . . ? C14 C13 C18 117.6(4) . . ? C15 C14 C13 121.5(4) . . ? N5 C12 N6 110.5(4) . . ? N5 C12 S2 123.0(4) . . ? N6 C12 S2 126.5(4) . . ? N5 C11 C10 109.4(4) . . ? C16 C15 C14 119.0(5) . . ? C17 C18 C13 120.5(5) . . ? C17 C16 C15 120.3(5) . . ? C17 C16 N7 119.9(5) . . ? C15 C16 N7 119.8(5) . . ? C18 C17 C16 121.1(5) . . ? N1 C10 C11 114.1(4) . . ? C12 N6 C13 134.7(4) . . ? C12 N5 C11 125.3(4) . . ? O4 N7 O3 123.3(5) . . ? O4 N7 C16 119.3(6) . . ? O3 N7 C16 117.4(5) . . ? N8 C21 N9 110.7(4) . . ? N8 C21 S3 122.7(3) . . ? N9 C21 S3 126.6(3) . . ? N8 C20 C19 110.3(4) . . ? N1 C19 C20 114.3(4) . . ? C23 C22 C27 117.8(4) . . ? C23 C22 N9 127.8(4) . . ? C27 C22 N9 114.4(4) . . ? C26 C25 C24 120.1(4) . . ? C26 C25 N10 118.8(5) . . ? C24 C25 N10 121.1(5) . . ? C26 C27 C22 121.2(4) . . ? C25 C26 C27 119.5(4) . . ? C23 C24 C25 120.4(5) . . ? C24 C23 C22 121.0(4) . . ? C21 N9 C22 132.9(4) . . ? C21 N8 C20 124.8(4) . . ? O6 N10 O5 122.8(5) . . ? O6 N10 C25 119.3(5) . . ? O5 N10 C25 117.9(5) . . ? C37 N11 C28 111.1(4) . . ? C37 N11 C46 110.8(4) . . ? C28 N11 C46 111.4(4) . . ? C32 C31 C36 119.2(4) . . ? C32 C31 N13 126.4(4) . . ? C36 C31 N13 114.4(4) . . ? C31 C36 C35 120.6(4) . . ? N12 C30 N13 111.1(4) . . ? N12 C30 S4 121.8(3) . . ? N13 C30 S4 127.0(4) . . ? C33 C34 C35 120.8(4) . . ? C33 C34 N14 119.3(5) . . ? C35 C34 N14 119.8(5) . . ? N12 C29 C28 110.3(4) . . ? C31 C32 C33 120.3(4) . . ? C34 C35 C36 119.0(4) . . ? C34 C33 C32 119.9(4) . . ? N11 C28 C29 114.0(4) . . ? C30 N13 C31 134.0(4) . . ? C30 N12 C29 125.2(4) . . ? O7 N14 O8 121.2(5) . . ? O7 N14 C34 120.6(5) . . ? O8 N14 C34 118.2(5) . . ? C45 C40 N16 127.3(4) . . ? C45 C40 C41 118.1(4) . . ? N16 C40 C41 114.6(4) . . ? C42 C41 C40 122.0(4) . . ? N15 C39 N16 110.6(4) . . ? N15 C39 S5 122.8(3) . . ? N16 C39 S5 126.6(3) . . ? C41 C42 C43 118.7(4) . . ? C44 C45 C40 120.5(4) . . ? C44 C43 C42 119.9(4) . . ? C44 C43 N17 121.2(5) . . ? C42 C43 N17 118.8(5) . . ? N15 C38 C37 108.7(4) . . ? C45 C44 C43 120.8(4) . . ? N11 C37 C38 114.0(4) . . ? C39 N16 C40 134.4(4) . . ? C39 N15 C38 125.1(4) . . ? O10 N17 O9 121.9(5) . . ? O10 N17 C43 118.6(5) . . ? O9 N17 C43 119.5(5) . . ? C54 C49 N19 127.6(4) . . ? C54 C49 C50 118.2(4) . . ? N19 C49 C50 114.3(4) . . ? C51 C50 C49 122.2(5) . . ? N18 C48 N19 111.1(4) . . ? N18 C48 S6 122.5(4) . . ? N19 C48 S6 126.4(4) . . ? C52 C51 C50 118.4(5) . . ? C53 C54 C49 120.3(5) . . ? C51 C52 C53 120.8(5) . . ? C51 C52 N20 120.3(5) . . ? C53 C52 N20 118.9(5) . . ? N18 C47 C46 109.5(4) . . ? C54 C53 C52 120.1(5) . . ? N11 C46 C47 114.6(4) . . ? C48 N19 C49 133.3(4) . . ? C48 N18 C47 125.1(4) . . ? O12 N20 O11 122.0(5) . . ? O12 N20 C52 120.3(6) . . ? O11 N20 C52 117.7(6) . . ? N21 C56 C55 178.1(9) . . ? N22 C58 C57 177.8(7) . . ? C71 N23 C59 114.2(5) . . ? C71 N23 C67 109.3(5) . . ? C59 N23 C67 107.2(4) . . ? C71 N23 C63 108.6(5) . . ? C59 N23 C63 108.4(5) . . ? C67 N23 C63 109.0(5) . . ? C59 C60 C61 113.5(5) . . ? N23 C59 C60 119.3(5) . . ? C62 C61 C60 120.7(6) . . ? C63 C64 C65 117.9(9) . . ? C64 C63 N23 116.0(6) . . ? C66 C65 C64 117.3(9) . . ? C68 C67 N23 120.0(6) . . ? C70 C69 C68 117.0(6) . . ? C67 C68 C69 116.2(6) . . ? N23 C71 C72 124.7(6) . . ? C71 C72 C73 128.0(8) . . ? C74 C73 C72 100.6(14) . . ? C87 N24 C75 112.8(4) . . ? C87 N24 C79 109.2(4) . . ? C75 N24 C79 108.2(4) . . ? C87 N24 C83 108.9(4) . . ? C75 N24 C83 107.9(4) . . ? C79 N24 C83 109.8(4) . . ? C76 C75 N24 117.9(5) . . ? C78 C77 C76 115.9(5) . . ? C75 C76 C77 111.2(5) . . ? C80 C79 N24 117.6(5) . . ? C79 C80 C81 112.4(5) . . ? C82 C81 C80 115.3(6) . . ? N24 C87 C88 119.9(5) . . ? C84 C83 N24 116.3(5) . . ? C85 C84 C83 116.8(8) . . ? C87 C88 C89 117.5(6) . . ? C86 C85 C84 115.0(9) . . ? C90 C89 C88 116.5(16) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.710 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.089 # Attachment 'CCDC 819535.cif' data_Thiourea-PO4 _database_code_depnum_ccdc_archive 'CCDC 819535' #TrackingRef 'CCDC 819535.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C27 H30 N10 O6 S3), 3(C16 H36 N), 2(C2 H3 N), O4 P' _chemical_formula_sum 'C106 H174 N25 O16 P S6' _chemical_formula_weight 2278.09 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5840(7) _cell_length_b 16.0821(8) _cell_length_c 28.9547(15) _cell_angle_alpha 103.421(4) _cell_angle_beta 93.523(5) _cell_angle_gamma 92.808(4) _cell_volume 6128.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2961 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 21.42 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.924 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and onega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 92714 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.1784 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 28.46 _reflns_number_total 29779 _reflns_number_gt 24513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 29779 _refine_ls_number_parameters 1401 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2051 _refine_ls_R_factor_gt 0.0860 _refine_ls_wR_factor_ref 0.2499 _refine_ls_wR_factor_gt 0.2158 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.004 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 1.0434(3) -0.0675(2) 0.29901(14) 0.0467(9) Uani 1 1 d . . . C3 C 1.0459(3) 0.1996(3) 0.32140(15) 0.0382(10) Uani 1 1 d . . . C1 C 1.1279(3) -0.0037(3) 0.31025(18) 0.0479(11) Uani 1 1 d . . . H1A H 1.1883 -0.0318 0.3024 0.057 Uiso 1 1 calc R . . H1B H 1.1334 0.0227 0.3441 0.057 Uiso 1 1 calc R . . C2 C 1.1154(3) 0.0643(3) 0.28267(17) 0.0450(11) Uani 1 1 d . . . H2A H 1.1763 0.1001 0.2865 0.054 Uiso 1 1 calc R . . H2B H 1.1024 0.0372 0.2491 0.054 Uiso 1 1 calc R . . N3 N 0.9576(2) 0.2360(2) 0.32991(12) 0.0401(8) Uani 1 1 d . . . H3 H 0.9053 0.2042 0.3178 0.048 Uiso 1 1 calc R . . N2 N 1.0350(3) 0.1173(2) 0.29870(13) 0.0424(9) Uani 1 1 d . . . H2 H 0.9759 0.0938 0.2931 0.051 Uiso 1 1 calc R . . C4 C 0.9421(3) 0.3189(3) 0.35594(15) 0.0393(10) Uani 1 1 d . . . C8 C 0.8423(4) 0.4404(3) 0.36454(17) 0.0488(12) Uani 1 1 d . . . H8 H 0.7918 0.4690 0.3531 0.059 Uiso 1 1 calc R . . C9 C 0.8676(3) 0.3618(3) 0.33844(15) 0.0395(10) Uani 1 1 d . . . H9 H 0.8344 0.3376 0.3090 0.047 Uiso 1 1 calc R . . C7 C 0.8924(4) 0.4745(3) 0.40698(19) 0.0636(15) Uani 1 1 d . . . C5 C 0.9931(4) 0.3551(3) 0.39943(17) 0.0540(13) Uani 1 1 d . . . H5 H 1.0435 0.3268 0.4111 0.065 Uiso 1 1 calc R . . C6 C 0.9684(4) 0.4334(3) 0.42519(19) 0.0697(17) Uani 1 1 d . . . H6 H 1.0020 0.4587 0.4544 0.084 Uiso 1 1 calc R . . N4 N 0.8660(5) 0.5561(3) 0.4360(2) 0.100(2) Uani 1 1 d . . . O1 O 0.9083(4) 0.5851(3) 0.47505(17) 0.123(2) Uani 1 1 d . . . O2 O 0.8014(4) 0.5927(3) 0.41881(18) 0.128(2) Uani 1 1 d . . . S1 S 1.15493(9) 0.25666(8) 0.33463(5) 0.0524(3) Uani 1 1 d . . . C10 C 1.0243(4) -0.1062(3) 0.3389(2) 0.0604(14) Uani 1 1 d . . . H10A H 1.0862 -0.1085 0.3570 0.073 Uiso 1 1 calc R . . H10B H 0.9966 -0.1645 0.3266 0.073 Uiso 1 1 calc R . . C11 C 0.9533(4) -0.0560(4) 0.37172(19) 0.0625(14) Uani 1 1 d . . . H11A H 0.9471 -0.0806 0.3991 0.075 Uiso 1 1 calc R . . H11B H 0.9799 0.0028 0.3832 0.075 Uiso 1 1 calc R . . C12 C 0.7844(3) -0.1181(3) 0.34510(17) 0.0481(12) Uani 1 1 d . . . N6 N 0.6982(3) -0.1019(2) 0.32287(13) 0.0410(9) Uani 1 1 d . . . H6A H 0.6975 -0.0534 0.3152 0.049 Uiso 1 1 calc R . . N5 N 0.8566(3) -0.0572(2) 0.34746(13) 0.0469(9) Uani 1 1 d . . . H5A H 0.8449 -0.0163 0.3337 0.056 Uiso 1 1 calc R . . S2 S 0.79625(11) -0.20404(10) 0.36896(6) 0.0782(5) Uani 1 1 d . . . C18 C 0.5221(3) -0.1155(3) 0.31479(15) 0.0430(11) Uani 1 1 d . . . H18 H 0.5224 -0.0563 0.3255 0.052 Uiso 1 1 calc R . . C13 C 0.6110(3) -0.1547(3) 0.31114(15) 0.0392(10) Uani 1 1 d . . . C17 C 0.4332(4) -0.1634(3) 0.30271(17) 0.0513(12) Uani 1 1 d . . . H17 H 0.3736 -0.1373 0.3058 0.062 Uiso 1 1 calc R . . C14 C 0.6083(4) -0.2430(3) 0.29262(19) 0.0568(13) Uani 1 1 d . . . H14 H 0.6671 -0.2702 0.2884 0.068 Uiso 1 1 calc R . . C16 C 0.4346(4) -0.2500(3) 0.28610(18) 0.0560(13) Uani 1 1 d . . . C15 C 0.5196(5) -0.2901(3) 0.2806(2) 0.0699(16) Uani 1 1 d . . . H15 H 0.5181 -0.3491 0.2687 0.084 Uiso 1 1 calc R . . N7 N 0.3413(5) -0.3022(5) 0.2740(2) 0.0943(18) Uani 1 1 d . . . O3 O 0.2643(4) -0.2640(4) 0.2776(2) 0.1108(17) Uani 1 1 d . . . O4 O 0.3425(4) -0.3801(4) 0.2607(3) 0.148(3) Uani 1 1 d . . . C19 C 1.0517(3) -0.1315(3) 0.25444(19) 0.0510(12) Uani 1 1 d . . . H19A H 1.0865 -0.1792 0.2610 0.061 Uiso 1 1 calc R . . H19B H 1.0894 -0.1062 0.2332 0.061 Uiso 1 1 calc R . . C20 C 0.9502(4) -0.1634(3) 0.23076(19) 0.0549(13) Uani 1 1 d . . . H20A H 0.9561 -0.2117 0.2041 0.066 Uiso 1 1 calc R . . H20B H 0.9101 -0.1827 0.2533 0.066 Uiso 1 1 calc R . . C21 C 0.9040(3) -0.0876(3) 0.16927(18) 0.0474(12) Uani 1 1 d . . . N9 N 0.8527(3) -0.0202(2) 0.16108(13) 0.0446(9) Uani 1 1 d . . . H9A H 0.8228 0.0071 0.1847 0.054 Uiso 1 1 calc R . . N8 N 0.9021(3) -0.0960(2) 0.21387(14) 0.0450(9) Uani 1 1 d . . . H8A H 0.8711 -0.0600 0.2336 0.054 Uiso 1 1 calc R . . S3 S 0.95916(13) -0.15447(10) 0.12671(6) 0.0806(5) Uani 1 1 d . . . C22 C 0.8425(3) 0.0102(3) 0.11962(15) 0.0426(11) Uani 1 1 d . . . C27 C 0.7546(3) 0.0460(3) 0.11104(15) 0.0418(10) Uani 1 1 d . . . H27 H 0.7045 0.0450 0.1314 0.050 Uiso 1 1 calc R . . C23 C 0.9176(4) 0.0130(3) 0.08872(18) 0.0578(13) Uani 1 1 d . . . H23 H 0.9778 -0.0095 0.0942 0.069 Uiso 1 1 calc R . . C26 C 0.7397(4) 0.0828(3) 0.07323(16) 0.0489(12) Uani 1 1 d . . . H26 H 0.6806 0.1074 0.0684 0.059 Uiso 1 1 calc R . . C24 C 0.9025(4) 0.0487(4) 0.05065(19) 0.0645(15) Uani 1 1 d . . . H24 H 0.9524 0.0500 0.0302 0.077 Uiso 1 1 calc R . . C25 C 0.8130(4) 0.0830(3) 0.04228(16) 0.0501(12) Uani 1 1 d . . . N10 N 0.7977(4) 0.1219(3) 0.00239(15) 0.0625(12) Uani 1 1 d . . . O5 O 0.8631(3) 0.1165(3) -0.02599(15) 0.0919(13) Uani 1 1 d . . . O6 O 0.7213(4) 0.1586(3) -0.00182(14) 0.0807(12) Uani 1 1 d . . . N11 N 0.4701(2) 0.2350(2) 0.25847(12) 0.0364(8) Uani 1 1 d . . . C29 C 0.5157(3) 0.1918(3) 0.17565(16) 0.0424(10) Uani 1 1 d . . . H29A H 0.4810 0.1369 0.1738 0.051 Uiso 1 1 calc R . . H29B H 0.5059 0.2054 0.1448 0.051 Uiso 1 1 calc R . . C28 C 0.4722(3) 0.2600(3) 0.21297(15) 0.0423(11) Uani 1 1 d . . . H28A H 0.5114 0.3137 0.2175 0.051 Uiso 1 1 calc R . . H28B H 0.4055 0.2687 0.2019 0.051 Uiso 1 1 calc R . . C30 C 0.6909(3) 0.2367(3) 0.17543(15) 0.0379(10) Uani 1 1 d . . . N12 N 0.6206(2) 0.1855(2) 0.18640(12) 0.0368(8) Uani 1 1 d . . . H12 H 0.6382 0.1466 0.2006 0.044 Uiso 1 1 calc R . . N13 N 0.7828(2) 0.2243(2) 0.19501(12) 0.0372(8) Uani 1 1 d . . . H13 H 0.7823 0.2069 0.2209 0.045 Uiso 1 1 calc R . . S4 S 0.66902(10) 0.30896(8) 0.14308(5) 0.0558(3) Uani 1 1 d . . . C31 C 0.8747(3) 0.2355(2) 0.17948(15) 0.0370(10) Uani 1 1 d . . . C33 C 1.0495(3) 0.2196(3) 0.19408(17) 0.0499(12) Uani 1 1 d . . . H33 H 1.1011 0.2044 0.2124 0.060 Uiso 1 1 calc R . . C32 C 0.9535(3) 0.2121(3) 0.20600(15) 0.0417(10) Uani 1 1 d . . . H32 H 0.9408 0.1909 0.2324 0.050 Uiso 1 1 calc R . . C36 C 0.8960(3) 0.2636(3) 0.13889(15) 0.0447(11) Uani 1 1 d . . . H36 H 0.8448 0.2772 0.1197 0.054 Uiso 1 1 calc R . . C34 C 1.0680(3) 0.2500(3) 0.15470(17) 0.0494(12) Uani 1 1 d . . . C35 C 0.9911(4) 0.2712(3) 0.12706(17) 0.0510(12) Uani 1 1 d . . . H35 H 1.0043 0.2909 0.1002 0.061 Uiso 1 1 calc R . . N14 N 1.1689(4) 0.2632(3) 0.14257(17) 0.0650(12) Uani 1 1 d . . . O8 O 1.2351(3) 0.2336(3) 0.16332(15) 0.0781(11) Uani 1 1 d . . . O7 O 1.1827(3) 0.3043(3) 0.11229(15) 0.0856(13) Uani 1 1 d . . . C38 C 0.5874(3) 0.3386(3) 0.31307(16) 0.0439(11) Uani 1 1 d . . . H38A H 0.6199 0.3457 0.2852 0.053 Uiso 1 1 calc R . . H38B H 0.5909 0.3939 0.3356 0.053 Uiso 1 1 calc R . . C37 C 0.4805(3) 0.3090(3) 0.29873(16) 0.0416(10) Uani 1 1 d . . . H37A H 0.4502 0.2945 0.3256 0.050 Uiso 1 1 calc R . . H37B H 0.4459 0.3555 0.2904 0.050 Uiso 1 1 calc R . . C39 C 0.6406(3) 0.2786(3) 0.38020(17) 0.0486(12) Uani 1 1 d . . . N15 N 0.6393(2) 0.2780(2) 0.33455(13) 0.0404(9) Uani 1 1 d . . . H15A H 0.6708 0.2398 0.3164 0.048 Uiso 1 1 calc R . . N16 N 0.6831(3) 0.2073(3) 0.38977(13) 0.0532(11) Uani 1 1 d . . . H16 H 0.6971 0.1700 0.3650 0.064 Uiso 1 1 calc R . . S5 S 0.59044(11) 0.35579(9) 0.42027(5) 0.0665(4) Uani 1 1 d . . . C45 C 0.7327(4) 0.1023(4) 0.42952(19) 0.0714(17) Uani 1 1 d . . . H45 H 0.7353 0.0653 0.3998 0.086 Uiso 1 1 calc R . . C40 C 0.7069(4) 0.1858(3) 0.43277(17) 0.0581(14) Uani 1 1 d . . . C44 C 0.7546(5) 0.0736(4) 0.4705(2) 0.0794(19) Uani 1 1 d . . . H44 H 0.7729 0.0180 0.4684 0.095 Uiso 1 1 calc R . . C42 C 0.7274(5) 0.2117(4) 0.51855(19) 0.082(2) Uani 1 1 d . . . H42 H 0.7264 0.2486 0.5484 0.099 Uiso 1 1 calc R . . C41 C 0.7071(5) 0.2396(4) 0.47762(19) 0.0748(18) Uani 1 1 d . . . H41 H 0.6930 0.2965 0.4802 0.090 Uiso 1 1 calc R . . C43 C 0.7488(5) 0.1288(4) 0.51394(19) 0.0766(19) Uani 1 1 d . . . N17 N 0.7674(4) 0.0973(4) 0.55760(19) 0.0904(17) Uani 1 1 d . . . O9 O 0.7941(4) 0.0238(4) 0.55332(16) 0.1104(18) Uani 1 1 d . . . O10 O 0.7534(4) 0.1455(4) 0.59583(15) 0.1067(17) Uani 1 1 d . . . C46 C 0.3852(3) 0.1766(3) 0.25925(16) 0.0415(10) Uani 1 1 d . . . H46A H 0.3629 0.1470 0.2269 0.050 Uiso 1 1 calc R . . H46B H 0.3316 0.2092 0.2731 0.050 Uiso 1 1 calc R . . C47 C 0.4104(3) 0.1112(3) 0.28792(16) 0.0420(10) Uani 1 1 d . . . H47A H 0.4382 0.1409 0.3194 0.050 Uiso 1 1 calc R . . H47B H 0.3503 0.0789 0.2916 0.050 Uiso 1 1 calc R . . C48 C 0.4559(3) -0.0196(3) 0.23162(15) 0.0362(10) Uani 1 1 d . . . N19 N 0.5388(2) -0.0589(2) 0.21409(12) 0.0354(8) Uani 1 1 d . . . H19 H 0.5919 -0.0257 0.2203 0.043 Uiso 1 1 calc R . . N18 N 0.4809(2) 0.0519(2) 0.26503(12) 0.0364(8) Uani 1 1 d . . . H18A H 0.5427 0.0640 0.2737 0.044 Uiso 1 1 calc R . . C49 C 0.5535(3) -0.1409(3) 0.18860(14) 0.0357(9) Uani 1 1 d . . . C52 C 0.6036(3) -0.3003(3) 0.13802(15) 0.0372(10) Uani 1 1 d . . . C54 C 0.4806(3) -0.2078(3) 0.17117(15) 0.0394(10) Uani 1 1 d . . . H54 H 0.4147 -0.1990 0.1765 0.047 Uiso 1 1 calc R . . C51 C 0.6775(3) -0.2367(3) 0.15575(17) 0.0468(11) Uani 1 1 d . . . H51 H 0.7433 -0.2467 0.1509 0.056 Uiso 1 1 calc R . . C50 C 0.6518(3) -0.1585(3) 0.18057(17) 0.0455(11) Uani 1 1 d . . . H50 H 0.7013 -0.1156 0.1925 0.055 Uiso 1 1 calc R . . C53 C 0.5068(3) -0.2866(3) 0.14609(16) 0.0415(10) Uani 1 1 d . . . H53 H 0.4584 -0.3307 0.1346 0.050 Uiso 1 1 calc R . . N20 N 0.6317(3) -0.3823(2) 0.11126(13) 0.0467(9) Uani 1 1 d . . . O11 O 0.7191(3) -0.3974(2) 0.11103(12) 0.0595(9) Uani 1 1 d . . . O12 O 0.5647(3) -0.4333(2) 0.08853(12) 0.0571(9) Uani 1 1 d . . . P1 P 0.75003(7) 0.08345(6) 0.27373(4) 0.0296(2) Uani 1 1 d . . . O13 O 0.84506(18) 0.03867(16) 0.28109(9) 0.0329(6) Uani 1 1 d . . . O16 O 0.67568(18) 0.06782(16) 0.30949(9) 0.0326(6) Uani 1 1 d . . . O14 O 0.70391(19) 0.04795(16) 0.22243(9) 0.0327(6) Uani 1 1 d . . . O15 O 0.77518(18) 0.18020(15) 0.28094(9) 0.0311(6) Uani 1 1 d . . . N21 N 0.5737(3) 0.6945(2) 0.97741(12) 0.0435(9) Uani 1 1 d . . . C55 C 0.6671(3) 0.6862(3) 1.00612(17) 0.0502(12) Uani 1 1 d . . . H55A H 0.6821 0.6264 0.9989 0.060 Uiso 1 1 calc R . . H55B H 0.6552 0.7024 1.0396 0.060 Uiso 1 1 calc R . . C56 C 0.7565(4) 0.7389(4) 0.9981(2) 0.0779(18) Uani 1 1 d . . . H56A H 0.7530 0.7980 1.0154 0.093 Uiso 1 1 calc R . . H56B H 0.7574 0.7378 0.9644 0.093 Uiso 1 1 calc R . . C58 C 0.9422(6) 0.7521(8) 1.0058(3) 0.174(5) Uani 1 1 d . . . H58A H 0.9371 0.7586 0.9736 0.261 Uiso 1 1 calc R . . H58B H 0.9990 0.7209 1.0105 0.261 Uiso 1 1 calc R . . H58C H 0.9490 0.8075 1.0274 0.261 Uiso 1 1 calc R . . C57 C 0.8506(4) 0.7036(5) 1.0149(3) 0.110(3) Uani 1 1 d . . . H57A H 0.8501 0.7068 1.0487 0.132 Uiso 1 1 calc R . . H57B H 0.8520 0.6438 0.9986 0.132 Uiso 1 1 calc R . . C59 C 0.5482(4) 0.7871(3) 0.98662(17) 0.0491(12) Uani 1 1 d . . . H59A H 0.4909 0.7906 0.9656 0.059 Uiso 1 1 calc R . . H59B H 0.6027 0.8199 0.9778 0.059 Uiso 1 1 calc R . . C60 C 0.5263(4) 0.8299(3) 1.03721(17) 0.0535(12) Uani 1 1 d . . . H60A H 0.4678 0.8017 1.0458 0.064 Uiso 1 1 calc R . . H60B H 0.5813 0.8249 1.0592 0.064 Uiso 1 1 calc R . . C61 C 0.5098(4) 0.9238(3) 1.04078(19) 0.0582(13) Uani 1 1 d . . . H61A H 0.5690 0.9518 1.0326 0.070 Uiso 1 1 calc R . . H61B H 0.4561 0.9283 1.0180 0.070 Uiso 1 1 calc R . . C62 C 0.4853(5) 0.9692(3) 1.0902(2) 0.0734(16) Uani 1 1 d . . . H62A H 0.4293 0.9395 1.0992 0.110 Uiso 1 1 calc R . . H62B H 0.4700 1.0269 1.0903 0.110 Uiso 1 1 calc R . . H62C H 0.5410 0.9701 1.1124 0.110 Uiso 1 1 calc R . . C64 C 0.3910(3) 0.6404(3) 0.97104(18) 0.0480(11) Uani 1 1 d . . . H64A H 0.3889 0.6142 0.9372 0.058 Uiso 1 1 calc R . . H64B H 0.3729 0.6991 0.9748 0.058 Uiso 1 1 calc R . . C63 C 0.4941(3) 0.6401(3) 0.99299(16) 0.0429(11) Uani 1 1 d . . . H63A H 0.5132 0.5814 0.9861 0.051 Uiso 1 1 calc R . . H63B H 0.4927 0.6589 1.0273 0.051 Uiso 1 1 calc R . . C65 C 0.3173(4) 0.5919(3) 0.9942(2) 0.0607(14) Uani 1 1 d . . . H65A H 0.3342 0.5327 0.9890 0.073 Uiso 1 1 calc R . . H65B H 0.3227 0.6163 1.0282 0.073 Uiso 1 1 calc R . . C66 C 0.2117(5) 0.5939(4) 0.9753(3) 0.096(2) Uani 1 1 d . . . H66A H 0.1925 0.6519 0.9825 0.144 Uiso 1 1 calc R . . H66B H 0.1693 0.5597 0.9900 0.144 Uiso 1 1 calc R . . H66C H 0.2060 0.5714 0.9414 0.144 Uiso 1 1 calc R . . C67 C 0.5839(3) 0.6650(3) 0.92412(15) 0.0478(11) Uani 1 1 d . . . H67A H 0.6271 0.7068 0.9146 0.057 Uiso 1 1 calc R . . H67B H 0.5194 0.6644 0.9076 0.057 Uiso 1 1 calc R . . C68 C 0.6244(4) 0.5766(3) 0.90759(17) 0.0568(13) Uani 1 1 d . . . H68A H 0.6899 0.5770 0.9230 0.068 Uiso 1 1 calc R . . H68B H 0.5822 0.5343 0.9172 0.068 Uiso 1 1 calc R . . C69 C 0.6299(4) 0.5515(4) 0.85438(19) 0.0753(17) Uani 1 1 d D . . H69A H 0.6725 0.5044 0.8468 0.090 Uiso 1 1 calc R . . H69B H 0.6603 0.5995 0.8442 0.090 Uiso 1 1 calc R . . C70 C 0.5315(4) 0.5253(4) 0.8262(2) 0.0807(18) Uani 1 1 d D . . H70A H 0.5004 0.4779 0.8360 0.121 Uiso 1 1 calc R . . H70B H 0.5417 0.5085 0.7929 0.121 Uiso 1 1 calc R . . H70C H 0.4900 0.5726 0.8318 0.121 Uiso 1 1 calc R . . N22 N 0.3299(3) 0.2448(3) 0.47788(15) 0.0581(11) Uani 1 1 d . . . C71 C 0.3689(5) 0.1620(4) 0.4503(2) 0.0807(18) Uani 1 1 d . . . H71A H 0.3606 0.1214 0.4700 0.097 Uiso 1 1 calc R . . H71B H 0.3225 0.1418 0.4226 0.097 Uiso 1 1 calc R . . C72 C 0.4704(7) 0.1493(7) 0.4318(4) 0.143(3) Uani 1 1 d . . . H72A H 0.5208 0.1647 0.4581 0.172 Uiso 1 1 calc R . . H72B H 0.4822 0.1857 0.4100 0.172 Uiso 1 1 calc R . . C73 C 0.4753(8) 0.0548(5) 0.4060(3) 0.142(4) Uani 1 1 d . . . H73A H 0.4150 0.0382 0.3855 0.170 Uiso 1 1 calc R . . H73B H 0.5294 0.0516 0.3855 0.170 Uiso 1 1 calc R . . C74 C 0.4884(6) -0.0128(5) 0.4349(3) 0.115(3) Uani 1 1 d . . . H74A H 0.5387 0.0078 0.4603 0.173 Uiso 1 1 calc R . . H74B H 0.5076 -0.0646 0.4145 0.173 Uiso 1 1 calc R . . H74C H 0.4272 -0.0240 0.4479 0.173 Uiso 1 1 calc R . . C76 C 0.1499(5) 0.1871(4) 0.4513(2) 0.0838(19) Uani 1 1 d . . . H76A H 0.1672 0.1303 0.4353 0.101 Uiso 1 1 calc R . . H76B H 0.1495 0.2224 0.4284 0.101 Uiso 1 1 calc R . . C75 C 0.2259(4) 0.2243(3) 0.4911(2) 0.0663(16) Uani 1 1 d . . . H75A H 0.2307 0.1846 0.5116 0.080 Uiso 1 1 calc R . . H75B H 0.2022 0.2767 0.5096 0.080 Uiso 1 1 calc R . . C78 C 0.0350(6) 0.1201(5) 0.5004(3) 0.119(3) Uani 1 1 d . . . H78A H 0.0529 0.0644 0.4842 0.178 Uiso 1 1 calc R . . H78B H -0.0325 0.1166 0.5082 0.178 Uiso 1 1 calc R . . H78C H 0.0772 0.1401 0.5291 0.178 Uiso 1 1 calc R . . C77 C 0.0467(5) 0.1809(5) 0.4689(3) 0.101(2) Uani 1 1 d . . . H77A H 0.0312 0.2374 0.4862 0.121 Uiso 1 1 calc R . . H77B H -0.0009 0.1632 0.4416 0.121 Uiso 1 1 calc R . . C79 C 0.3985(8) 0.2868(4) 0.5219(3) 0.147(4) Uani 1 1 d D . . H79A H 0.4562 0.3110 0.5104 0.177 Uiso 1 1 calc R . . H79B H 0.3649 0.3348 0.5394 0.177 Uiso 1 1 calc R . . N23 N 0.0009(3) 0.5418(2) 0.23028(14) 0.0517(10) Uani 1 1 d . . . C82 C 0.0356(4) 0.6181(3) 0.2711(2) 0.0617(14) Uani 1 1 d . . . H82A H 0.1068 0.6269 0.2712 0.074 Uiso 1 1 calc R . . H82B H 0.0070 0.6687 0.2645 0.074 Uiso 1 1 calc R . . C83 C 0.0111(4) 0.6116(3) 0.3200(2) 0.0677(15) Uani 1 1 d . . . H83A H 0.0204 0.5539 0.3236 0.081 Uiso 1 1 calc R . . H83B H -0.0577 0.6230 0.3242 0.081 Uiso 1 1 calc R . . C84 C 0.0764(5) 0.6748(4) 0.35743(19) 0.085(2) Uani 1 1 d D . . H84A H 0.0738 0.7311 0.3507 0.102 Uiso 1 1 calc R . . H84B H 0.1441 0.6586 0.3554 0.102 Uiso 1 1 calc R . . C85 C 0.0472(6) 0.6801(6) 0.4075(2) 0.121(3) Uani 1 1 d D . . H85A H 0.0888 0.7235 0.4294 0.181 Uiso 1 1 calc R . . H85B H 0.0546 0.6259 0.4153 0.181 Uiso 1 1 calc R . . H85C H -0.0205 0.6944 0.4095 0.181 Uiso 1 1 calc R . . C86 C 0.0231(4) 0.5673(3) 0.1843(2) 0.0609(14) Uani 1 1 d . . . H86A H -0.0108 0.6184 0.1829 0.073 Uiso 1 1 calc R . . H86B H 0.0934 0.5817 0.1853 0.073 Uiso 1 1 calc R . . C87 C -0.0067(5) 0.4992(4) 0.13896(19) 0.0769(17) Uani 1 1 d D . . H87A H 0.0154 0.4449 0.1434 0.092 Uiso 1 1 calc R . . H87B H -0.0783 0.4935 0.1348 0.092 Uiso 1 1 calc R . . C88 C 0.0321(6) 0.5145(5) 0.0937(2) 0.109(2) Uani 1 1 d D . . H88A H 0.1037 0.5212 0.0972 0.131 Uiso 1 1 calc R . . H88B H 0.0127 0.4656 0.0675 0.131 Uiso 1 1 calc R . . C89 C -0.0088(6) 0.5941(5) 0.0830(3) 0.129(3) Uani 1 1 d D . . H89A H -0.0796 0.5898 0.0827 0.194 Uiso 1 1 calc R . . H89B H 0.0101 0.6000 0.0524 0.194 Uiso 1 1 calc R . . H89C H 0.0171 0.6434 0.1070 0.194 Uiso 1 1 calc R . . C90 C 0.0553(4) 0.4635(3) 0.23494(19) 0.0558(13) Uani 1 1 d . . . H90A H 0.0225 0.4138 0.2128 0.067 Uiso 1 1 calc R . . H90B H 0.0492 0.4553 0.2668 0.067 Uiso 1 1 calc R . . C91 C 0.1645(4) 0.4662(3) 0.2260(2) 0.0633(14) Uani 1 1 d . . . H91A H 0.1911 0.5253 0.2343 0.076 Uiso 1 1 calc R . . H91B H 0.1715 0.4436 0.1924 0.076 Uiso 1 1 calc R . . C92 C 0.2237(4) 0.4148(3) 0.25465(17) 0.0704(16) Uani 1 1 d D . . H92A H 0.1885 0.3596 0.2516 0.085 Uiso 1 1 calc R . . H92B H 0.2868 0.4044 0.2411 0.085 Uiso 1 1 calc R . . C93 C 0.2422(5) 0.4580(4) 0.30684(17) 0.0842(18) Uani 1 1 d D . . H93A H 0.2801 0.5113 0.3103 0.126 Uiso 1 1 calc R . . H93B H 0.2780 0.4215 0.3228 0.126 Uiso 1 1 calc R . . H93C H 0.1801 0.4686 0.3206 0.126 Uiso 1 1 calc R . . C94 C -0.1085(3) 0.5192(2) 0.23085(18) 0.0483(11) Uani 1 1 d D . . H94A H -0.1273 0.4703 0.2046 0.058 Uiso 1 1 calc R . . H94B H -0.1193 0.5017 0.2601 0.058 Uiso 1 1 calc R . . C96 C -0.2841(4) 0.5561(3) 0.22276(18) 0.0559(13) Uani 1 1 d . . . H96A H -0.3256 0.6014 0.2183 0.067 Uiso 1 1 calc R . . H96B H -0.2955 0.5093 0.1947 0.067 Uiso 1 1 calc R . . C95 C -0.1760(3) 0.5896(3) 0.22723(19) 0.0564(13) Uani 1 1 d D . . H95A H -0.1621 0.6115 0.1997 0.068 Uiso 1 1 calc R . . H95B H -0.1639 0.6363 0.2553 0.068 Uiso 1 1 calc R . . C97 C -0.3142(4) 0.5252(4) 0.2656(2) 0.0664(15) Uani 1 1 d . . . H97A H -0.2825 0.4737 0.2668 0.100 Uiso 1 1 calc R . . H97B H -0.3846 0.5140 0.2632 0.100 Uiso 1 1 calc R . . H97C H -0.2946 0.5685 0.2941 0.100 Uiso 1 1 calc R . . C98 C 0.3312(5) 0.3068(3) 0.4459(2) 0.095(2) Uani 1 1 d D . . H98A H 0.3987 0.3151 0.4379 0.114 Uiso 1 1 calc R . . H98B H 0.2921 0.2803 0.4165 0.114 Uiso 1 1 calc R . . C99 C 0.2935(6) 0.3938(3) 0.4655(3) 0.134(4) Uani 1 1 d D . . H99A H 0.3322 0.4227 0.4946 0.161 Uiso 1 1 calc R . . H99B H 0.2250 0.3879 0.4726 0.161 Uiso 1 1 calc R . . C101 C 0.2701(9) 0.5339(4) 0.4441(4) 0.195(6) Uani 1 1 d D . . H10C H 0.2230 0.5350 0.4676 0.292 Uiso 1 1 calc R . . H10D H 0.2402 0.5518 0.4174 0.292 Uiso 1 1 calc R . . H10E H 0.3264 0.5721 0.4577 0.292 Uiso 1 1 calc R . . C100 C 0.3029(7) 0.4441(4) 0.4278(3) 0.161(5) Uani 1 1 d D . . H10F H 0.3712 0.4468 0.4200 0.193 Uiso 1 1 calc R . . H10G H 0.2630 0.4147 0.3992 0.193 Uiso 1 1 calc R . . C104 C 0.1989(5) 0.0287(4) 0.1238(2) 0.0772(17) Uani 1 1 d . . . H10H H 0.1646 -0.0261 0.1104 0.116 Uiso 1 1 calc R . . H10I H 0.1535 0.0678 0.1395 0.116 Uiso 1 1 calc R . . H10J H 0.2512 0.0225 0.1463 0.116 Uiso 1 1 calc R . . C105 C 0.2402(5) 0.0618(4) 0.0861(3) 0.0776(17) Uani 1 1 d . . . N25 N 0.2716(6) 0.0862(4) 0.0562(3) 0.120(2) Uani 1 1 d . . . C106 C 0.2162(5) 0.7787(4) 0.1092(2) 0.0728(16) Uani 1 1 d . . . H10K H 0.2454 0.7715 0.0793 0.109 Uiso 1 1 calc R . . H10L H 0.2450 0.8300 0.1307 0.109 Uiso 1 1 calc R . . H10M H 0.1463 0.7831 0.1043 0.109 Uiso 1 1 calc R . . C107 C 0.2336(4) 0.7085(5) 0.1283(3) 0.086(2) Uani 1 1 d . . . N26 N 0.2473(5) 0.6513(5) 0.1439(4) 0.164(4) Uani 1 1 d . . . C109 C 0.4697(7) 0.3869(6) 0.6187(3) 0.142(4) Uani 1 1 d D . . H10N H 0.4580 0.4233 0.5972 0.213 Uiso 1 1 calc R . . H10O H 0.5181 0.4150 0.6437 0.213 Uiso 1 1 calc R . . H10P H 0.4092 0.3753 0.6322 0.213 Uiso 1 1 calc R . . C108 C 0.5072(6) 0.3038(7) 0.5921(3) 0.196(6) Uani 1 1 d D . . H10Q H 0.5350 0.2753 0.6155 0.235 Uiso 1 1 calc R . . H10R H 0.5611 0.3179 0.5742 0.235 Uiso 1 1 calc R . . S11 S 0.33849(8) -0.05443(8) 0.21310(4) 0.0482(3) Uani 1 1 d . . . C110 C 0.4363(7) 0.2395(5) 0.5580(3) 0.198(6) Uani 1 1 d D . . H11C H 0.4699 0.1897 0.5427 0.238 Uiso 1 1 calc R . . H11D H 0.3824 0.2209 0.5745 0.238 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 0.029(2) 0.048(2) 0.067(3) 0.022(2) 0.0004(17) 0.0038(16) C3 0.035(2) 0.041(3) 0.039(3) 0.008(2) 0.0074(18) -0.0016(18) C1 0.030(2) 0.053(3) 0.060(3) 0.011(2) 0.003(2) 0.001(2) C2 0.031(2) 0.040(3) 0.063(3) 0.007(2) 0.014(2) 0.0008(19) N3 0.0261(19) 0.039(2) 0.049(2) -0.0010(16) 0.0031(15) -0.0026(15) N2 0.0264(19) 0.038(2) 0.063(3) 0.0095(18) 0.0079(16) 0.0015(15) C4 0.037(2) 0.045(3) 0.036(3) 0.007(2) 0.0074(19) 0.0032(19) C8 0.052(3) 0.041(3) 0.050(3) 0.006(2) -0.008(2) 0.010(2) C9 0.039(3) 0.040(2) 0.036(2) 0.0040(19) -0.0003(19) -0.0028(19) C7 0.074(4) 0.045(3) 0.059(3) -0.014(2) -0.015(3) 0.021(3) C5 0.054(3) 0.056(3) 0.046(3) -0.002(2) -0.004(2) 0.017(2) C6 0.076(4) 0.067(4) 0.050(3) -0.018(3) -0.023(3) 0.027(3) N4 0.122(5) 0.074(3) 0.081(4) -0.028(3) -0.041(3) 0.053(3) O1 0.155(5) 0.097(3) 0.080(3) -0.049(3) -0.054(3) 0.070(3) O2 0.163(5) 0.084(3) 0.104(4) -0.038(3) -0.066(3) 0.078(3) S1 0.0332(6) 0.0554(8) 0.0593(8) -0.0035(6) 0.0056(5) -0.0107(5) C10 0.037(3) 0.073(4) 0.083(4) 0.047(3) -0.009(3) 0.002(2) C11 0.042(3) 0.096(4) 0.058(3) 0.042(3) -0.008(2) -0.007(3) C12 0.042(3) 0.053(3) 0.057(3) 0.028(2) 0.004(2) 0.002(2) N6 0.041(2) 0.035(2) 0.052(2) 0.0227(17) 0.0008(17) -0.0014(16) N5 0.036(2) 0.057(2) 0.054(2) 0.0294(19) -0.0015(17) -0.0031(18) S2 0.0534(9) 0.0898(11) 0.1150(13) 0.0757(10) -0.0032(8) -0.0003(7) C18 0.046(3) 0.040(3) 0.044(3) 0.011(2) 0.004(2) 0.002(2) C13 0.040(3) 0.037(3) 0.042(3) 0.014(2) 0.0058(19) -0.0022(19) C17 0.040(3) 0.068(4) 0.053(3) 0.027(3) 0.004(2) -0.002(2) C14 0.057(3) 0.035(3) 0.080(4) 0.018(2) 0.008(3) 0.003(2) C16 0.057(4) 0.058(3) 0.055(3) 0.025(3) -0.005(2) -0.022(3) C15 0.072(4) 0.041(3) 0.094(5) 0.015(3) 0.004(3) -0.014(3) N7 0.067(4) 0.114(5) 0.101(5) 0.038(4) -0.012(3) -0.037(4) O3 0.063(3) 0.140(4) 0.131(4) 0.050(3) -0.014(3) -0.049(3) O4 0.120(5) 0.074(4) 0.240(8) 0.039(4) -0.025(4) -0.060(3) C19 0.035(3) 0.039(3) 0.080(4) 0.017(2) 0.001(2) 0.012(2) C20 0.052(3) 0.036(3) 0.075(4) 0.010(2) -0.003(3) 0.005(2) C21 0.034(3) 0.043(3) 0.057(3) -0.005(2) 0.000(2) 0.005(2) N9 0.038(2) 0.052(2) 0.041(2) 0.0032(18) 0.0073(16) 0.0098(17) N8 0.037(2) 0.039(2) 0.056(3) 0.0030(18) 0.0023(17) 0.0074(16) S3 0.0831(11) 0.0783(10) 0.0722(10) -0.0089(8) 0.0174(8) 0.0394(9) C22 0.037(3) 0.051(3) 0.033(3) -0.003(2) 0.0024(19) 0.000(2) C27 0.038(3) 0.049(3) 0.036(3) 0.002(2) 0.0058(19) 0.002(2) C23 0.042(3) 0.082(4) 0.049(3) 0.010(3) 0.011(2) 0.017(3) C26 0.046(3) 0.050(3) 0.043(3) -0.004(2) -0.001(2) 0.001(2) C24 0.053(3) 0.088(4) 0.050(3) 0.007(3) 0.021(3) -0.001(3) C25 0.053(3) 0.055(3) 0.037(3) 0.003(2) 0.006(2) -0.008(2) N10 0.076(4) 0.067(3) 0.041(3) 0.007(2) 0.010(2) -0.013(3) O5 0.089(3) 0.124(4) 0.066(3) 0.031(2) 0.019(2) -0.015(3) O6 0.093(3) 0.086(3) 0.066(3) 0.022(2) 0.006(2) 0.012(2) N11 0.0294(19) 0.037(2) 0.043(2) 0.0093(16) 0.0081(15) 0.0053(15) C29 0.035(3) 0.046(3) 0.046(3) 0.013(2) 0.0000(19) 0.0026(19) C28 0.036(3) 0.044(3) 0.049(3) 0.015(2) 0.003(2) 0.0085(19) C30 0.038(3) 0.038(2) 0.039(3) 0.0108(19) 0.0085(19) 0.0034(19) N12 0.036(2) 0.039(2) 0.038(2) 0.0121(16) 0.0063(15) 0.0068(15) N13 0.033(2) 0.040(2) 0.042(2) 0.0136(16) 0.0090(15) 0.0006(15) S4 0.0518(8) 0.0599(8) 0.0669(9) 0.0346(7) 0.0099(6) 0.0122(6) C31 0.038(3) 0.033(2) 0.036(2) 0.0020(18) 0.0074(19) -0.0026(18) C33 0.037(3) 0.064(3) 0.044(3) 0.005(2) 0.002(2) -0.004(2) C32 0.037(3) 0.051(3) 0.038(3) 0.013(2) 0.0081(19) -0.002(2) C36 0.045(3) 0.050(3) 0.037(3) 0.008(2) 0.003(2) -0.010(2) C34 0.039(3) 0.060(3) 0.042(3) 0.000(2) 0.008(2) -0.018(2) C35 0.054(3) 0.060(3) 0.038(3) 0.011(2) 0.010(2) -0.013(2) N14 0.050(3) 0.089(3) 0.045(3) -0.003(2) 0.010(2) -0.020(2) O8 0.038(2) 0.115(3) 0.074(3) 0.009(2) 0.0043(19) -0.008(2) O7 0.064(3) 0.124(4) 0.065(3) 0.018(3) 0.021(2) -0.031(2) C38 0.047(3) 0.038(2) 0.047(3) 0.009(2) 0.008(2) 0.005(2) C37 0.039(3) 0.039(2) 0.047(3) 0.007(2) 0.010(2) 0.0115(19) C39 0.035(3) 0.062(3) 0.046(3) 0.005(2) 0.005(2) 0.013(2) N15 0.036(2) 0.041(2) 0.043(2) 0.0062(17) 0.0080(16) 0.0069(16) N16 0.054(3) 0.063(3) 0.041(2) 0.0039(19) 0.0049(18) 0.028(2) S5 0.0741(10) 0.0789(10) 0.0460(8) 0.0043(7) 0.0123(7) 0.0417(8) C45 0.087(4) 0.083(4) 0.045(3) 0.008(3) 0.007(3) 0.048(3) C40 0.061(3) 0.073(3) 0.040(3) 0.005(2) 0.003(2) 0.038(3) C44 0.098(5) 0.095(4) 0.051(4) 0.018(3) 0.002(3) 0.059(4) C42 0.092(5) 0.113(5) 0.037(3) 0.000(3) -0.004(3) 0.054(4) C41 0.088(4) 0.084(4) 0.052(4) 0.008(3) -0.003(3) 0.049(3) C43 0.085(4) 0.108(5) 0.042(3) 0.020(3) 0.003(3) 0.052(4) N17 0.090(4) 0.130(5) 0.056(4) 0.027(3) -0.002(3) 0.050(4) O9 0.142(5) 0.133(4) 0.070(3) 0.042(3) 0.000(3) 0.069(4) O10 0.122(4) 0.163(5) 0.036(2) 0.017(3) -0.002(2) 0.057(3) C46 0.030(2) 0.049(3) 0.045(3) 0.009(2) 0.0060(19) 0.0057(19) C47 0.031(2) 0.049(3) 0.045(3) 0.007(2) 0.0093(19) 0.0031(19) C48 0.029(2) 0.040(2) 0.040(3) 0.013(2) 0.0027(18) -0.0001(18) N19 0.0251(18) 0.0354(19) 0.044(2) 0.0074(16) 0.0026(15) -0.0033(14) N18 0.0255(18) 0.040(2) 0.043(2) 0.0073(17) 0.0018(15) 0.0030(15) C49 0.042(3) 0.034(2) 0.031(2) 0.0099(18) 0.0006(18) 0.0013(18) C52 0.040(3) 0.033(2) 0.039(3) 0.0088(19) 0.0040(19) -0.0010(18) C54 0.035(2) 0.035(2) 0.047(3) 0.007(2) 0.0051(19) -0.0033(18) C51 0.038(3) 0.044(3) 0.054(3) 0.003(2) 0.006(2) 0.000(2) C50 0.033(3) 0.038(3) 0.059(3) -0.002(2) 0.006(2) -0.0045(19) C53 0.040(3) 0.031(2) 0.050(3) 0.007(2) 0.000(2) -0.0094(18) N20 0.058(3) 0.039(2) 0.044(2) 0.0109(18) 0.012(2) -0.003(2) O11 0.050(2) 0.049(2) 0.075(2) 0.0016(17) 0.0134(17) 0.0116(16) O12 0.061(2) 0.0423(19) 0.063(2) 0.0043(17) 0.0068(18) -0.0099(16) P1 0.0256(5) 0.0299(6) 0.0329(6) 0.0066(4) 0.0037(4) 0.0005(4) O13 0.0265(15) 0.0322(15) 0.0401(16) 0.0090(12) 0.0008(12) 0.0017(11) O16 0.0263(15) 0.0361(15) 0.0361(16) 0.0096(12) 0.0072(11) -0.0016(11) O14 0.0298(15) 0.0338(15) 0.0332(16) 0.0052(12) 0.0046(11) 0.0004(11) O15 0.0276(15) 0.0288(14) 0.0361(16) 0.0059(12) 0.0056(11) -0.0009(11) N21 0.045(2) 0.048(2) 0.038(2) 0.0146(17) 0.0038(17) -0.0057(17) C55 0.045(3) 0.063(3) 0.041(3) 0.010(2) 0.001(2) -0.002(2) C56 0.058(4) 0.121(5) 0.048(3) 0.012(3) 0.008(3) -0.023(3) C58 0.059(5) 0.349(15) 0.067(5) -0.031(7) 0.016(4) -0.058(7) C57 0.041(4) 0.170(7) 0.083(5) -0.037(5) -0.006(3) -0.013(4) C59 0.055(3) 0.041(3) 0.054(3) 0.018(2) 0.007(2) -0.006(2) C60 0.066(3) 0.046(3) 0.049(3) 0.013(2) 0.003(2) -0.002(2) C61 0.066(4) 0.046(3) 0.062(3) 0.012(2) 0.006(3) -0.008(2) C62 0.082(4) 0.057(3) 0.078(4) 0.007(3) 0.015(3) 0.001(3) C64 0.045(3) 0.044(3) 0.058(3) 0.016(2) 0.006(2) 0.003(2) C63 0.050(3) 0.043(3) 0.040(3) 0.018(2) 0.009(2) 0.001(2) C65 0.055(3) 0.061(3) 0.066(4) 0.012(3) 0.022(3) -0.003(2) C66 0.054(4) 0.104(5) 0.118(6) 0.007(4) 0.018(4) -0.021(3) C67 0.044(3) 0.063(3) 0.036(3) 0.014(2) 0.007(2) -0.012(2) C68 0.063(3) 0.056(3) 0.049(3) 0.010(2) 0.012(2) -0.016(2) C69 0.080(4) 0.085(4) 0.057(4) 0.009(3) 0.021(3) -0.018(3) C70 0.090(5) 0.090(4) 0.064(4) 0.021(3) 0.010(3) 0.002(4) N22 0.071(3) 0.051(3) 0.052(3) 0.016(2) -0.009(2) 0.002(2) C71 0.066(4) 0.096(5) 0.082(4) 0.015(3) 0.033(3) 0.021(3) C72 0.113(8) 0.185(10) 0.134(8) 0.044(7) 0.021(6) 0.000(6) C73 0.206(10) 0.071(5) 0.121(7) -0.030(5) -0.045(6) 0.065(6) C74 0.122(7) 0.139(7) 0.076(5) 0.001(5) 0.001(4) 0.046(5) C76 0.080(5) 0.092(5) 0.094(5) 0.041(4) 0.030(4) 0.028(4) C75 0.078(4) 0.063(3) 0.060(4) 0.008(3) 0.020(3) 0.032(3) C78 0.119(7) 0.139(7) 0.124(7) 0.068(6) 0.046(5) 0.040(5) C77 0.086(5) 0.107(5) 0.128(6) 0.055(5) 0.037(4) 0.017(4) C79 0.262(12) 0.068(5) 0.113(6) 0.026(4) -0.049(7) 0.081(6) N23 0.058(3) 0.040(2) 0.059(3) 0.018(2) 0.004(2) -0.0083(18) C82 0.063(4) 0.041(3) 0.076(4) 0.011(3) -0.010(3) -0.011(2) C83 0.070(4) 0.059(3) 0.069(4) 0.005(3) -0.004(3) 0.013(3) C84 0.105(5) 0.062(4) 0.075(5) -0.004(3) -0.025(4) 0.016(3) C85 0.101(6) 0.154(7) 0.088(6) -0.015(5) -0.001(4) 0.044(5) C86 0.054(3) 0.061(3) 0.078(4) 0.038(3) 0.006(3) -0.008(2) C87 0.080(4) 0.094(5) 0.062(4) 0.030(4) 0.007(3) -0.006(3) C88 0.091(6) 0.122(6) 0.119(7) 0.044(5) 0.002(5) -0.018(5) C89 0.087(6) 0.152(8) 0.143(8) 0.020(6) 0.030(5) -0.003(5) C90 0.059(3) 0.043(3) 0.067(3) 0.014(2) 0.012(3) 0.003(2) C91 0.053(3) 0.063(3) 0.077(4) 0.021(3) 0.011(3) 0.003(3) C92 0.060(4) 0.065(4) 0.086(5) 0.011(3) 0.022(3) 0.008(3) C93 0.082(5) 0.070(4) 0.092(5) 0.005(4) -0.004(4) 0.002(3) C94 0.052(3) 0.040(3) 0.054(3) 0.016(2) 0.006(2) -0.008(2) C96 0.063(4) 0.053(3) 0.050(3) 0.010(2) 0.002(2) 0.004(2) C95 0.058(3) 0.047(3) 0.064(3) 0.015(2) 0.002(3) 0.003(2) C97 0.055(3) 0.069(4) 0.085(4) 0.036(3) 0.013(3) 0.007(3) C98 0.094(5) 0.077(5) 0.125(6) 0.063(4) -0.030(4) -0.019(4) C99 0.138(7) 0.065(5) 0.203(10) 0.067(6) -0.070(7) -0.013(4) C101 0.247(15) 0.075(6) 0.247(14) 0.046(7) -0.108(11) -0.020(7) C100 0.164(9) 0.085(6) 0.243(12) 0.099(7) -0.104(8) -0.030(5) C104 0.074(4) 0.080(4) 0.084(4) 0.033(3) -0.001(3) 0.000(3) C105 0.079(5) 0.060(4) 0.096(5) 0.025(4) 0.001(4) -0.004(3) N25 0.148(7) 0.086(4) 0.133(6) 0.036(4) 0.047(5) -0.012(4) C106 0.069(4) 0.067(4) 0.082(4) 0.022(3) -0.004(3) 0.003(3) C107 0.051(4) 0.088(5) 0.133(6) 0.062(4) -0.019(3) -0.010(3) N26 0.079(5) 0.155(7) 0.294(11) 0.148(8) -0.040(6) -0.029(4) C109 0.117(7) 0.241(11) 0.053(5) 0.006(6) 0.002(4) 0.008(7) C108 0.095(7) 0.384(18) 0.053(5) -0.058(8) -0.025(4) 0.040(9) S11 0.0294(6) 0.0545(7) 0.0565(8) 0.0067(6) -0.0007(5) -0.0008(5) C110 0.273(17) 0.190(11) 0.143(10) 0.026(9) 0.091(10) 0.098(12) _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 C10 1.465(6) . ? N1 C19 1.466(6) . ? N1 C1 1.470(6) . ? C3 N2 1.330(5) . ? C3 N3 1.372(5) . ? C3 S1 1.678(4) . ? C1 C2 1.506(6) . ? C2 N2 1.452(5) . ? N3 C4 1.404(5) . ? C4 C5 1.385(6) . ? C4 C9 1.387(6) . ? C8 C7 1.350(7) . ? C8 C9 1.384(6) . ? C7 C6 1.393(7) . ? C7 N4 1.458(6) . ? C5 C6 1.375(6) . ? N4 O1 1.214(6) . ? N4 O2 1.224(6) . ? C10 C11 1.522(8) . ? C11 N5 1.448(6) . ? C12 N5 1.339(6) . ? C12 N6 1.367(5) . ? C12 S2 1.693(5) . ? N6 C13 1.399(5) . ? C18 C17 1.381(7) . ? C18 C13 1.388(6) . ? C13 C14 1.395(6) . ? C17 C16 1.365(7) . ? C14 C15 1.372(7) . ? C16 C15 1.350(8) . ? C16 N7 1.462(8) . ? N7 O4 1.223(8) . ? N7 O3 1.237(8) . ? C19 C20 1.511(7) . ? C20 N8 1.453(5) . ? C21 N8 1.331(6) . ? C21 N9 1.374(5) . ? C21 S3 1.678(5) . ? N9 C22 1.400(6) . ? C22 C27 1.384(6) . ? C22 C23 1.402(6) . ? C27 C26 1.369(6) . ? C23 C24 1.365(7) . ? C26 C25 1.380(7) . ? C24 C25 1.390(7) . ? C25 N10 1.445(6) . ? N10 O6 1.232(6) . ? N10 O5 1.239(6) . ? N11 C46 1.454(5) . ? N11 C37 1.455(5) . ? N11 C28 1.466(5) . ? C29 N12 1.453(5) . ? C29 C28 1.520(6) . ? C30 N12 1.331(5) . ? C30 N13 1.382(5) . ? C30 S4 1.680(4) . ? N13 C31 1.370(5) . ? C31 C36 1.394(6) . ? C31 C32 1.397(6) . ? C33 C34 1.372(7) . ? C33 C32 1.376(6) . ? C36 C35 1.364(6) . ? C34 C35 1.381(7) . ? C34 N14 1.453(6) . ? N14 O8 1.227(6) . ? N14 O7 1.232(6) . ? C38 N15 1.458(5) . ? C38 C37 1.508(6) . ? C39 N15 1.319(6) . ? C39 N16 1.385(6) . ? C39 S5 1.692(4) . ? N16 C40 1.391(6) . ? C45 C40 1.388(7) . ? C45 C44 1.389(7) . ? C40 C41 1.383(7) . ? C44 C43 1.370(7) . ? C42 C43 1.357(8) . ? C42 C41 1.378(8) . ? C43 N17 1.479(7) . ? N17 O10 1.226(6) . ? N17 O9 1.234(6) . ? C46 C47 1.523(6) . ? C47 N18 1.462(5) . ? C48 N18 1.334(5) . ? C48 N19 1.384(5) . ? C48 S11 1.677(4) . ? N19 C49 1.384(5) . ? C49 C50 1.400(6) . ? C49 C54 1.406(6) . ? C52 C53 1.369(6) . ? C52 C51 1.382(6) . ? C52 N20 1.448(5) . ? C54 C53 1.382(6) . ? C51 C50 1.369(6) . ? N20 O11 1.224(5) . ? N20 O12 1.239(5) . ? P1 O13 1.536(3) . ? P1 O15 1.539(3) . ? P1 O16 1.543(3) . ? P1 O14 1.543(3) . ? N21 C55 1.503(6) . ? N21 C59 1.511(5) . ? N21 C63 1.513(6) . ? N21 C67 1.523(6) . ? C55 C56 1.508(7) . ? C56 C57 1.522(9) . ? C58 C57 1.506(11) . ? C59 C60 1.521(7) . ? C60 C61 1.518(6) . ? C61 C62 1.513(7) . ? C64 C63 1.503(6) . ? C64 C65 1.520(7) . ? C65 C66 1.508(8) . ? C67 C68 1.531(7) . ? C68 C69 1.507(7) . ? C69 C70 1.5092(10) . ? N22 C98 1.510(7) . ? N22 C71 1.523(7) . ? N22 C75 1.525(7) . ? N22 C79 1.531(9) . ? C71 C72 1.516(11) . ? C72 C73 1.537(11) . ? C73 C74 1.527(11) . ? C76 C75 1.491(9) . ? C76 C77 1.528(9) . ? C78 C77 1.493(9) . ? C79 C110 1.5090(10) . ? N23 C94 1.514(6) . ? N23 C90 1.520(6) . ? N23 C86 1.523(6) . ? N23 C82 1.525(6) . ? C82 C83 1.502(8) . ? C83 C84 1.509(8) . ? C84 C85 1.5097(10) . ? C86 C87 1.519(8) . ? C87 C88 1.5104(10) . ? C88 C89 1.5089(10) . ? C90 C91 1.521(7) . ? C91 C92 1.524(7) . ? C92 C93 1.5097(10) . ? C94 C95 1.5095(10) . ? C96 C97 1.511(7) . ? C96 C95 1.525(7) . ? C98 C99 1.5101(10) . ? C99 C100 1.5105(10) . ? C101 C100 1.5096(10) . ? C104 C105 1.451(10) . ? C105 N25 1.127(8) . ? C106 C107 1.393(8) . ? C107 N26 1.133(8) . ? C109 C108 1.5099(10) . ? C108 C110 1.5107(10) . ? 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 C10 N1 C19 112.7(4) . . ? C10 N1 C1 112.3(4) . . ? C19 N1 C1 112.4(4) . . ? N2 C3 N3 113.0(4) . . ? N2 C3 S1 124.5(3) . . ? N3 C3 S1 122.4(3) . . ? N1 C1 C2 110.7(4) . . ? N2 C2 C1 111.6(4) . . ? C3 N3 C4 127.9(4) . . ? C3 N2 C2 124.8(4) . . ? C5 C4 C9 120.2(4) . . ? C5 C4 N3 122.1(4) . . ? C9 C4 N3 117.6(4) . . ? C7 C8 C9 118.5(4) . . ? C8 C9 C4 120.5(4) . . ? C8 C7 C6 122.2(4) . . ? C8 C7 N4 120.0(4) . . ? C6 C7 N4 117.7(5) . . ? C6 C5 C4 119.3(4) . . ? C5 C6 C7 119.2(5) . . ? O1 N4 O2 123.1(5) . . ? O1 N4 C7 120.0(5) . . ? O2 N4 C7 116.9(5) . . ? N1 C10 C11 111.8(4) . . ? N5 C11 C10 111.4(4) . . ? N5 C12 N6 112.8(4) . . ? N5 C12 S2 124.0(3) . . ? N6 C12 S2 123.2(4) . . ? C12 N6 C13 127.9(3) . . ? C12 N5 C11 123.9(4) . . ? C17 C18 C13 120.7(4) . . ? C18 C13 C14 118.3(4) . . ? C18 C13 N6 117.6(4) . . ? C14 C13 N6 123.9(4) . . ? C16 C17 C18 118.6(4) . . ? C15 C14 C13 120.5(5) . . ? C15 C16 C17 122.4(5) . . ? C15 C16 N7 118.1(6) . . ? C17 C16 N7 119.5(6) . . ? C16 C15 C14 119.4(5) . . ? O4 N7 O3 123.3(6) . . ? O4 N7 C16 119.5(7) . . ? O3 N7 C16 117.2(6) . . ? N1 C19 C20 110.3(4) . . ? N8 C20 C19 110.8(4) . . ? N8 C21 N9 113.1(4) . . ? N8 C21 S3 123.7(3) . . ? N9 C21 S3 123.2(4) . . ? C21 N9 C22 129.0(4) . . ? C21 N8 C20 123.0(4) . . ? C27 C22 N9 116.9(4) . . ? C27 C22 C23 118.4(4) . . ? N9 C22 C23 124.5(4) . . ? C26 C27 C22 121.5(4) . . ? C24 C23 C22 120.2(4) . . ? C27 C26 C25 119.6(4) . . ? C23 C24 C25 120.4(4) . . ? C26 C25 C24 119.8(5) . . ? C26 C25 N10 119.8(5) . . ? C24 C25 N10 120.4(5) . . ? O6 N10 O5 123.3(5) . . ? O6 N10 C25 119.1(4) . . ? O5 N10 C25 117.6(5) . . ? C46 N11 C37 113.7(3) . . ? C46 N11 C28 112.0(3) . . ? C37 N11 C28 111.8(3) . . ? N12 C29 C28 112.2(4) . . ? N11 C28 C29 111.2(3) . . ? N12 C30 N13 111.6(3) . . ? N12 C30 S4 123.8(3) . . ? N13 C30 S4 124.7(3) . . ? C30 N12 C29 123.5(3) . . ? C31 N13 C30 129.9(4) . . ? N13 C31 C36 126.5(4) . . ? N13 C31 C32 115.9(4) . . ? C36 C31 C32 117.5(4) . . ? C34 C33 C32 119.0(4) . . ? C33 C32 C31 121.9(4) . . ? C35 C36 C31 120.7(4) . . ? C33 C34 C35 120.3(4) . . ? C33 C34 N14 120.5(5) . . ? C35 C34 N14 119.1(5) . . ? C36 C35 C34 120.6(4) . . ? O8 N14 O7 124.0(5) . . ? O8 N14 C34 118.2(5) . . ? O7 N14 C34 117.8(5) . . ? N15 C38 C37 112.0(4) . . ? N11 C37 C38 111.9(3) . . ? N15 C39 N16 111.6(4) . . ? N15 C39 S5 122.6(3) . . ? N16 C39 S5 125.8(4) . . ? C39 N15 C38 123.7(3) . . ? C39 N16 C40 130.8(4) . . ? C40 C45 C44 120.3(5) . . ? C41 C40 C45 118.1(5) . . ? C41 C40 N16 126.1(4) . . ? C45 C40 N16 115.9(4) . . ? C43 C44 C45 118.9(5) . . ? C43 C42 C41 118.0(5) . . ? C42 C41 C40 122.1(5) . . ? C42 C43 C44 122.5(5) . . ? C42 C43 N17 118.5(5) . . ? C44 C43 N17 119.0(5) . . ? O10 N17 O9 124.0(5) . . ? O10 N17 C43 117.8(5) . . ? O9 N17 C43 118.2(5) . . ? N11 C46 C47 111.5(3) . . ? N18 C47 C46 112.0(3) . . ? N18 C48 N19 111.2(3) . . ? N18 C48 S11 123.3(3) . . ? N19 C48 S11 125.4(3) . . ? C48 N19 C49 133.0(4) . . ? C48 N18 C47 124.4(3) . . ? N19 C49 C50 115.8(4) . . ? N19 C49 C54 126.7(4) . . ? C50 C49 C54 117.5(4) . . ? C53 C52 C51 121.0(4) . . ? C53 C52 N20 120.9(4) . . ? C51 C52 N20 118.1(4) . . ? C53 C54 C49 120.0(4) . . ? C50 C51 C52 118.6(4) . . ? C51 C50 C49 122.3(4) . . ? C52 C53 C54 120.5(4) . . ? O11 N20 O12 123.2(4) . . ? O11 N20 C52 119.4(4) . . ? O12 N20 C52 117.3(4) . . ? O13 P1 O15 109.38(15) . . ? O13 P1 O16 109.86(15) . . ? O15 P1 O16 109.92(14) . . ? O13 P1 O14 109.58(14) . . ? O15 P1 O14 108.45(14) . . ? O16 P1 O14 109.62(15) . . ? C55 N21 C59 110.5(4) . . ? C55 N21 C63 106.0(3) . . ? C59 N21 C63 111.0(3) . . ? C55 N21 C67 111.9(3) . . ? C59 N21 C67 106.6(3) . . ? C63 N21 C67 110.8(3) . . ? N21 C55 C56 115.4(4) . . ? C55 C56 C57 110.2(6) . . ? C58 C57 C56 112.2(8) . . ? N21 C59 C60 116.9(4) . . ? C61 C60 C59 109.8(4) . . ? C62 C61 C60 112.0(4) . . ? C63 C64 C65 111.1(4) . . ? C64 C63 N21 116.9(3) . . ? C66 C65 C64 113.5(5) . . ? N21 C67 C68 115.6(4) . . ? C69 C68 C67 112.1(4) . . ? C68 C69 C70 114.7(5) . . ? C98 N22 C71 107.0(4) . . ? C98 N22 C75 112.4(4) . . ? C71 N22 C75 108.1(4) . . ? C98 N22 C79 105.9(5) . . ? C71 N22 C79 111.6(5) . . ? C75 N22 C79 111.7(6) . . ? C72 C71 N22 127.5(6) . . ? C71 C72 C73 108.6(8) . . ? C74 C73 C72 119.9(8) . . ? C75 C76 C77 111.9(6) . . ? C76 C75 N22 117.4(4) . . ? C78 C77 C76 114.2(6) . . ? C110 C79 N22 123.5(7) . . ? C94 N23 C90 107.4(3) . . ? C94 N23 C86 110.8(4) . . ? C90 N23 C86 110.5(4) . . ? C94 N23 C82 111.0(4) . . ? C90 N23 C82 110.3(4) . . ? C86 N23 C82 106.8(4) . . ? C83 C82 N23 116.4(4) . . ? C82 C83 C84 110.4(5) . . ? C83 C84 C85 113.4(6) . . ? C87 C86 N23 115.1(4) . . ? C88 C87 C86 116.5(5) . . ? C89 C88 C87 109.9(6) . . ? N23 C90 C91 116.2(4) . . ? C90 C91 C92 112.3(4) . . ? C93 C92 C91 113.9(4) . . ? C95 C94 N23 115.8(4) . . ? C97 C96 C95 113.2(4) . . ? C94 C95 C96 110.7(4) . . ? C99 C98 N22 116.6(5) . . ? C98 C99 C100 107.0(5) . . ? C101 C100 C99 111.9(6) . . ? N25 C105 C104 178.7(8) . . ? N26 C107 C106 179.7(8) . . ? C109 C108 C110 119.2(7) . . ? C79 C110 C108 104.7(7) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.141 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.077