# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Gopal Das' _publ_contact_author_email gdas@iitg.ernet.in loop_ _publ_author_name 'Sandeep Dey' 'Gopal Das' data_chloride _database_code_depnum_ccdc_archive 'CCDC 819536' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H31 N10 O6 S3, C3 H7 N O, Cl' _chemical_formula_sum 'C30 H38 Cl N11 O7 S3' _chemical_formula_weight 796.37 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' Cl Cl 0.1484 0.1585 '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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.2973(3) _cell_length_b 9.0007(4) _cell_length_c 12.7365(5) _cell_angle_alpha 98.535(3) _cell_angle_beta 98.527(2) _cell_angle_gamma 97.221(2) _cell_volume 919.58(6) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5121 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 18.62 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 0.336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.851 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details SADABS _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 omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13809 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.38 _reflns_number_total 4525 _reflns_number_gt 3422 _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 'Mercury 2.3' _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^)+(0.0764P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(5) _refine_ls_number_reflns 4525 _refine_ls_number_parameters 499 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S3 S 0.29037(9) 1.05874(10) 0.63540(7) 0.0520(2) Uani 1 1 d . . . Cl1 Cl 0.83584(8) 0.75201(8) 0.63978(6) 0.05032(19) Uani 1 1 d . . . S2 S 0.42258(9) 0.53904(10) 0.70619(8) 0.0601(2) Uani 1 1 d . . . C28 C 0.7192(7) 0.7536(6) 1.0877(4) 0.0801(12) Uani 1 1 d . . . H28A H 0.7583 0.8574 1.0840 0.120 Uiso 1 1 calc R . . H28B H 0.7861 0.7225 1.1463 0.120 Uiso 1 1 calc R . . H28C H 0.6068 0.7445 1.0990 0.120 Uiso 1 1 calc R . . C29 C 0.6929(7) 0.4946(5) 0.9822(4) 0.0839(13) Uani 1 1 d . . . H29A H 0.7024 0.4445 0.9119 0.126 Uiso 1 1 calc R . . H29B H 0.5829 0.4680 0.9953 0.126 Uiso 1 1 calc R . . H29C H 0.7698 0.4633 1.0355 0.126 Uiso 1 1 calc R . . N11 N 0.7288(3) 0.6581(3) 0.9880(2) 0.0526(6) Uani 1 1 d . . . C30 C 0.7692(3) 0.7180(4) 0.9053(3) 0.0481(7) Uani 1 1 d . . . H30 H 0.7758 0.6517 0.8432 0.058 Uiso 1 1 calc R . . O7 O 0.7988(3) 0.8550(3) 0.9041(2) 0.0634(6) Uani 1 1 d . . . N1 N 0.3084(2) 1.0298(3) 0.8932(2) 0.0353(5) Uani 1 1 d . . . C3 C -0.0581(3) 1.1884(3) 0.7266(2) 0.0376(6) Uani 1 1 d . . . C2 C 0.0543(3) 1.1565(3) 0.9121(2) 0.0403(6) Uani 1 1 d . . . H2A H 0.0093 1.0879 0.9561 0.048 Uiso 1 1 calc R . . H2B H 0.0225 1.2552 0.9336 0.048 Uiso 1 1 calc R . . C5 C -0.2808(4) 1.2533(4) 0.5208(3) 0.0537(8) Uani 1 1 d . . . H5 H -0.2752 1.3295 0.5797 0.064 Uiso 1 1 calc R . . C4 C -0.1971(3) 1.1319(3) 0.5310(2) 0.0390(6) Uani 1 1 d . . . C9 C -0.2059(4) 1.0186(4) 0.4412(3) 0.0525(7) Uani 1 1 d . . . H9 H -0.1478 0.9376 0.4474 0.063 Uiso 1 1 calc R . . C1 C 0.2408(3) 1.1711(3) 0.9336(2) 0.0396(6) Uani 1 1 d . . . H1A H 0.2857 1.2534 0.9001 0.048 Uiso 1 1 calc R . . H1B H 0.2788 1.1988 1.0107 0.048 Uiso 1 1 calc R . . C7 C -0.3804(4) 1.1471(4) 0.3363(3) 0.0498(7) Uani 1 1 d . . . C6 C -0.3730(5) 1.2616(4) 0.4227(3) 0.0623(9) Uani 1 1 d . . . H6 H -0.4294 1.3434 0.4150 0.075 Uiso 1 1 calc R . . C8 C -0.2988(4) 1.0257(4) 0.3447(3) 0.0521(8) Uani 1 1 d . . . H8 H -0.3063 0.9492 0.2857 0.063 Uiso 1 1 calc R . . N2 N -0.0165(3) 1.1004(3) 0.7999(2) 0.0388(5) Uani 1 1 d . . . N3 N -0.1097(3) 1.1025(3) 0.6263(2) 0.0467(6) Uani 1 1 d . . . N4 N -0.4795(4) 1.1524(4) 0.2328(3) 0.0690(9) Uani 1 1 d . . . O2 O -0.5131(4) 1.0379(4) 0.1656(2) 0.0840(9) Uani 1 1 d . . . O1 O -0.5231(7) 1.2708(5) 0.2160(3) 0.1297(18) Uani 1 1 d . . . S1 S -0.04389(12) 1.37555(9) 0.75501(7) 0.0616(3) Uani 1 1 d . . . C12 C 0.2520(3) 0.6180(3) 0.6860(2) 0.0374(6) Uani 1 1 d . . . C13 C 0.1216(3) 0.4976(3) 0.4962(2) 0.0389(6) Uani 1 1 d . . . C10 C 0.2389(3) 0.8901(3) 0.9335(2) 0.0414(6) Uani 1 1 d . . . H10A H 0.1199 0.8832 0.9243 0.050 Uiso 1 1 calc R . . H10B H 0.2805 0.9006 1.0099 0.050 Uiso 1 1 calc R . . C18 C 0.0041(4) 0.5244(4) 0.4131(3) 0.0526(8) Uani 1 1 d . . . H18 H -0.0460 0.6110 0.4233 0.063 Uiso 1 1 calc R . . C11 C 0.2821(4) 0.7441(4) 0.8757(3) 0.0487(7) Uani 1 1 d . . . H11A H 0.4007 0.7525 0.8802 0.058 Uiso 1 1 calc R . . H11B H 0.2457 0.6599 0.9103 0.058 Uiso 1 1 calc R . . C16 C 0.0393(4) 0.3013(4) 0.3022(3) 0.0515(8) Uani 1 1 d . . . C14 C 0.1988(4) 0.3690(4) 0.4783(3) 0.0528(8) Uani 1 1 d . . . H14 H 0.2779 0.3488 0.5320 0.063 Uiso 1 1 calc R . . C15 C 0.1570(5) 0.2722(4) 0.3805(3) 0.0619(9) Uani 1 1 d . . . H15 H 0.2089 0.1872 0.3678 0.074 Uiso 1 1 calc R . . C17 C -0.0389(4) 0.4259(4) 0.3168(3) 0.0551(8) Uani 1 1 d . . . H17 H -0.1192 0.4435 0.2628 0.066 Uiso 1 1 calc R . . N6 N 0.1478(3) 0.6031(3) 0.5905(2) 0.0417(5) Uani 1 1 d . . . N5 N 0.2037(3) 0.7149(3) 0.7636(2) 0.0402(5) Uani 1 1 d . . . N7 N -0.0073(5) 0.1940(4) 0.1999(3) 0.0717(9) Uani 1 1 d . . . O4 O -0.1256(5) 0.2138(4) 0.1354(3) 0.0962(11) Uani 1 1 d . . . O3 O 0.0686(6) 0.0881(4) 0.1837(3) 0.1112(13) Uani 1 1 d . . . C21 C 0.4517(3) 0.9637(3) 0.6467(2) 0.0382(6) Uani 1 1 d . . . C22 C 0.4116(3) 0.8033(3) 0.4621(2) 0.0403(6) Uani 1 1 d . . . C20 C 0.5734(3) 1.1069(4) 0.8280(3) 0.0470(7) Uani 1 1 d . . . H20A H 0.5216 1.1884 0.8020 0.056 Uiso 1 1 calc R . . H20B H 0.6891 1.1458 0.8541 0.056 Uiso 1 1 calc R . . C23 C 0.2903(4) 0.8665(4) 0.4030(3) 0.0539(8) Uani 1 1 d . . . H23 H 0.2513 0.9513 0.4353 0.065 Uiso 1 1 calc R . . C24 C 0.2281(5) 0.8041(5) 0.2971(3) 0.0607(9) Uani 1 1 d . . . H24 H 0.1473 0.8464 0.2579 0.073 Uiso 1 1 calc R . . C27 C 0.4691(4) 0.6782(4) 0.4112(3) 0.0527(8) Uani 1 1 d . . . H27 H 0.5506 0.6356 0.4494 0.063 Uiso 1 1 calc R . . C26 C 0.4079(5) 0.6158(4) 0.3049(3) 0.0584(8) Uani 1 1 d . . . H26 H 0.4482 0.5327 0.2713 0.070 Uiso 1 1 calc R . . C19 C 0.4951(3) 1.0614(4) 0.9198(3) 0.0458(7) Uani 1 1 d . . . H19A H 0.5278 1.1421 0.9818 0.055 Uiso 1 1 calc R . . H19B H 0.5358 0.9711 0.9392 0.055 Uiso 1 1 calc R . . C25 C 0.2862(4) 0.6791(4) 0.2498(3) 0.0525(7) Uani 1 1 d . . . N9 N 0.4859(3) 0.8588(3) 0.5682(2) 0.0423(5) Uani 1 1 d . . . N8 N 0.5598(3) 0.9831(3) 0.7393(2) 0.0468(6) Uani 1 1 d . . . N10 N 0.2167(5) 0.6104(5) 0.1387(3) 0.0715(9) Uani 1 1 d . . . O5 O 0.1017(5) 0.6631(5) 0.0924(3) 0.1020(12) Uani 1 1 d . . . O6 O 0.2783(6) 0.5088(6) 0.0946(3) 0.1208(16) Uani 1 1 d . . . H1N H 0.276(4) 1.023(4) 0.833(3) 0.052(10) Uiso 1 1 d . . . H3N H -0.090(6) 1.014(7) 0.622(4) 0.091(16) Uiso 1 1 d . . . H2N H -0.048(4) 1.016(5) 0.788(3) 0.050(10) Uiso 1 1 d . . . H6N H 0.071(7) 0.654(6) 0.601(4) 0.091(16) Uiso 1 1 d . . . H5N H 0.091(5) 0.721(4) 0.754(3) 0.046(9) Uiso 1 1 d . . . H9N H 0.564(4) 0.819(4) 0.588(3) 0.036(8) Uiso 1 1 d . . . H8N H 0.622(5) 0.922(5) 0.742(4) 0.064(12) Uiso 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 0.0543(4) 0.0637(5) 0.0483(4) 0.0129(4) 0.0159(3) 0.0353(4) Cl1 0.0431(3) 0.0530(4) 0.0552(5) 0.0026(3) 0.0038(3) 0.0219(3) S2 0.0434(4) 0.0602(5) 0.0694(6) -0.0064(4) -0.0087(4) 0.0227(3) C28 0.111(3) 0.074(3) 0.054(3) -0.001(2) 0.014(2) 0.021(2) C29 0.111(3) 0.050(2) 0.094(3) 0.012(2) 0.026(3) 0.012(2) N11 0.0595(15) 0.0436(14) 0.0523(17) 0.0023(12) 0.0047(12) 0.0108(11) C30 0.0394(14) 0.0473(16) 0.0529(19) -0.0029(14) 0.0010(12) 0.0097(11) O7 0.0718(15) 0.0459(12) 0.0697(17) 0.0073(12) 0.0074(12) 0.0072(11) N1 0.0314(10) 0.0438(12) 0.0269(12) -0.0005(9) -0.0012(8) 0.0068(8) C3 0.0293(11) 0.0444(14) 0.0368(15) 0.0005(12) 0.0049(10) 0.0057(10) C2 0.0363(12) 0.0475(15) 0.0354(15) -0.0026(12) 0.0049(10) 0.0125(10) C5 0.069(2) 0.0500(17) 0.0404(17) -0.0021(14) 0.0002(14) 0.0236(15) C4 0.0389(13) 0.0420(14) 0.0344(14) 0.0018(11) 0.0056(10) 0.0054(10) C9 0.0666(19) 0.0506(17) 0.0399(17) 0.0015(14) 0.0038(13) 0.0209(14) C1 0.0366(12) 0.0407(14) 0.0359(14) -0.0046(11) -0.0024(10) 0.0078(10) C7 0.0567(17) 0.0562(18) 0.0352(16) 0.0075(14) 0.0002(12) 0.0131(14) C6 0.081(2) 0.0555(19) 0.049(2) 0.0044(16) -0.0046(16) 0.0307(17) C8 0.0665(19) 0.0528(18) 0.0343(16) -0.0003(14) 0.0063(13) 0.0100(15) N2 0.0352(11) 0.0387(12) 0.0379(13) -0.0024(10) -0.0013(8) 0.0080(9) N3 0.0536(14) 0.0466(14) 0.0369(13) -0.0029(11) -0.0026(10) 0.0196(11) N4 0.081(2) 0.080(2) 0.0444(17) 0.0086(17) -0.0049(14) 0.0287(18) O2 0.104(2) 0.091(2) 0.0445(16) -0.0078(15) -0.0163(14) 0.0234(17) O1 0.203(5) 0.104(3) 0.073(2) 0.000(2) -0.044(3) 0.083(3) S1 0.0894(6) 0.0379(4) 0.0491(5) 0.0029(3) 0.0004(4) -0.0037(4) C12 0.0324(12) 0.0314(12) 0.0453(16) 0.0033(11) 0.0012(10) 0.0037(9) C13 0.0389(13) 0.0367(13) 0.0398(15) 0.0031(12) 0.0079(10) 0.0033(10) C10 0.0441(14) 0.0423(14) 0.0341(15) 0.0030(12) 0.0003(11) 0.0043(11) C18 0.0574(17) 0.0516(18) 0.0466(18) -0.0008(14) 0.0013(13) 0.0198(14) C11 0.0554(17) 0.0445(15) 0.0406(17) 0.0020(13) -0.0089(12) 0.0122(13) C16 0.0678(19) 0.0435(16) 0.0405(17) -0.0007(13) 0.0122(14) 0.0039(14) C14 0.0615(18) 0.0411(15) 0.052(2) 0.0015(14) -0.0011(14) 0.0149(13) C15 0.083(2) 0.0367(15) 0.064(2) -0.0017(15) 0.0083(18) 0.0207(15) C17 0.0632(19) 0.060(2) 0.0392(17) 0.0000(15) 0.0021(13) 0.0161(15) N6 0.0395(12) 0.0424(13) 0.0419(14) 0.0020(11) 0.0007(10) 0.0145(10) N5 0.0385(12) 0.0394(12) 0.0380(13) -0.0005(10) -0.0051(9) 0.0103(9) N7 0.103(3) 0.0560(18) 0.051(2) -0.0068(15) 0.0150(18) 0.0067(17) O4 0.122(3) 0.106(3) 0.0475(18) -0.0166(17) -0.0056(17) 0.026(2) O3 0.173(4) 0.072(2) 0.077(2) -0.0271(17) -0.004(2) 0.054(2) C21 0.0316(12) 0.0361(13) 0.0489(16) 0.0076(12) 0.0107(10) 0.0079(10) C22 0.0383(13) 0.0383(13) 0.0456(17) 0.0079(12) 0.0100(11) 0.0071(10) C20 0.0336(13) 0.0484(16) 0.0529(19) -0.0075(14) 0.0076(12) 0.0025(11) C23 0.0605(18) 0.0535(18) 0.0488(19) 0.0049(15) 0.0036(14) 0.0238(14) C24 0.066(2) 0.068(2) 0.051(2) 0.0134(17) 0.0015(15) 0.0252(17) C27 0.0580(18) 0.0478(17) 0.0517(19) -0.0001(15) 0.0040(14) 0.0222(14) C26 0.070(2) 0.0530(18) 0.053(2) 0.0005(16) 0.0129(16) 0.0186(16) C19 0.0287(12) 0.0546(17) 0.0479(17) -0.0012(14) -0.0035(10) 0.0065(11) C25 0.0624(19) 0.0519(17) 0.0422(17) 0.0074(14) 0.0081(14) 0.0063(14) N9 0.0381(12) 0.0439(13) 0.0454(14) 0.0012(11) 0.0053(10) 0.0181(10) N8 0.0367(12) 0.0506(15) 0.0501(16) -0.0053(12) 0.0054(10) 0.0143(11) N10 0.084(2) 0.081(2) 0.0466(19) 0.0040(17) 0.0071(16) 0.0134(18) O5 0.100(2) 0.142(3) 0.0566(19) -0.002(2) -0.0123(16) 0.041(2) O6 0.171(4) 0.123(3) 0.060(2) -0.024(2) -0.008(2) 0.071(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 1.677(3) . ? S2 C12 1.665(3) . ? C28 N11 1.443(5) . ? C29 N11 1.452(5) . ? N11 C30 1.320(5) . ? C30 O7 1.229(4) . ? N1 C1 1.506(4) . ? N1 C10 1.508(4) . ? N1 C19 1.517(3) . ? C3 N2 1.346(4) . ? C3 N3 1.369(4) . ? C3 S1 1.655(3) . ? C2 N2 1.451(4) . ? C2 C1 1.516(4) . ? C5 C4 1.378(5) . ? C5 C6 1.381(5) . ? C4 N3 1.396(4) . ? C4 C9 1.402(4) . ? C9 C8 1.365(5) . ? C7 C8 1.365(5) . ? C7 C6 1.379(5) . ? C7 N4 1.458(4) . ? N4 O1 1.206(5) . ? N4 O2 1.211(5) . ? C12 N5 1.360(4) . ? C12 N6 1.362(4) . ? C13 N6 1.387(4) . ? C13 C14 1.398(4) . ? C13 C18 1.399(5) . ? C10 C11 1.519(4) . ? C18 C17 1.373(5) . ? C11 N5 1.449(4) . ? C16 C15 1.367(5) . ? C16 C17 1.367(5) . ? C16 N7 1.471(4) . ? C14 C15 1.380(5) . ? N7 O3 1.216(5) . ? N7 O4 1.232(5) . ? C21 N8 1.346(4) . ? C21 N9 1.358(4) . ? C22 C27 1.388(4) . ? C22 N9 1.389(4) . ? C22 C23 1.397(4) . ? C20 N8 1.444(4) . ? C20 C19 1.503(5) . ? C23 C24 1.377(5) . ? C24 C25 1.372(5) . ? C27 C26 1.380(5) . ? C26 C25 1.375(5) . ? C25 N10 1.458(5) . ? N10 O6 1.210(6) . ? N10 O5 1.230(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 N11 C28 120.8(3) . . ? C30 N11 C29 121.5(3) . . ? C28 N11 C29 117.8(4) . . ? O7 C30 N11 124.9(3) . . ? C1 N1 C10 114.0(2) . . ? C1 N1 C19 108.8(2) . . ? C10 N1 C19 112.1(2) . . ? N2 C3 N3 110.9(3) . . ? N2 C3 S1 123.9(2) . . ? N3 C3 S1 125.2(2) . . ? N2 C2 C1 113.0(2) . . ? C4 C5 C6 119.9(3) . . ? C5 C4 N3 126.2(3) . . ? C5 C4 C9 119.3(3) . . ? N3 C4 C9 114.3(3) . . ? C8 C9 C4 120.8(3) . . ? N1 C1 C2 114.7(2) . . ? C8 C7 C6 121.9(3) . . ? C8 C7 N4 118.0(3) . . ? C6 C7 N4 120.1(3) . . ? C7 C6 C5 119.3(3) . . ? C7 C8 C9 118.8(3) . . ? C3 N2 C2 124.9(2) . . ? C3 N3 C4 132.7(3) . . ? O1 N4 O2 122.1(4) . . ? O1 N4 C7 119.1(3) . . ? O2 N4 C7 118.8(4) . . ? N5 C12 N6 110.6(3) . . ? N5 C12 S2 123.3(2) . . ? N6 C12 S2 125.9(2) . . ? N6 C13 C14 126.3(3) . . ? N6 C13 C18 115.3(3) . . ? C14 C13 C18 118.4(3) . . ? N1 C10 C11 113.2(2) . . ? C17 C18 C13 121.5(3) . . ? N5 C11 C10 110.3(2) . . ? C15 C16 C17 122.0(3) . . ? C15 C16 N7 119.2(3) . . ? C17 C16 N7 118.8(3) . . ? C15 C14 C13 119.6(3) . . ? C16 C15 C14 120.1(3) . . ? C16 C17 C18 118.4(3) . . ? C12 N6 C13 132.7(3) . . ? C12 N5 C11 123.5(3) . . ? O3 N7 O4 122.9(4) . . ? O3 N7 C16 119.2(4) . . ? O4 N7 C16 117.9(4) . . ? N8 C21 N9 113.1(3) . . ? N8 C21 S3 121.5(2) . . ? N9 C21 S3 125.4(2) . . ? C27 C22 N9 116.2(3) . . ? C27 C22 C23 118.4(3) . . ? N9 C22 C23 125.3(3) . . ? N8 C20 C19 113.1(3) . . ? C24 C23 C22 120.4(3) . . ? C25 C24 C23 119.5(3) . . ? C26 C27 C22 121.4(3) . . ? C25 C26 C27 118.6(3) . . ? C20 C19 N1 112.9(3) . . ? C24 C25 C26 121.6(3) . . ? C24 C25 N10 119.5(3) . . ? C26 C25 N10 118.9(3) . . ? C21 N9 C22 133.4(3) . . ? C21 N8 C20 124.7(3) . . ? O6 N10 O5 122.8(4) . . ? O6 N10 C25 119.0(4) . . ? O5 N10 C25 118.2(4) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.284 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.048 data_hydrogenphosphate _database_code_depnum_ccdc_archive 'CCDC 819537' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C27 H31 N10 O6 S3), H O4 P, 3(H2O)' _chemical_formula_sum 'C54 H69 N20 O19 P S6' _chemical_formula_weight 1518.63 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' 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 14.2058(8) _cell_length_b 15.0756(9) _cell_length_c 19.4881(11) _cell_angle_alpha 100.526(4) _cell_angle_beta 109.789(4) _cell_angle_gamma 100.260(4) _cell_volume 3728.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2352 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 15.41 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1578 _exptl_absorpt_coefficient_mu 0.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.891 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details SADABS _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 omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69613 _diffrn_reflns_av_R_equivalents 0.1140 _diffrn_reflns_av_sigmaI/netI 0.3793 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 28.46 _reflns_number_total 18459 _reflns_number_gt 14268 _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 'Mercury 2.3' _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. Appropriate bond restraints have been applied in SHELXL-97 to ensure standard bond geometry of the receptor cations and the lattice water molecules are refined isotropically due to disorder. The structure Contains Solvent Accessible VOIDS of 133 A3. ; _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^+0.3000P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18459 _refine_ls_number_parameters 903 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.3243 _refine_ls_R_factor_gt 0.0956 _refine_ls_wR_factor_ref 0.2413 _refine_ls_wR_factor_gt 0.2104 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.013 _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 0.38538(18) 0.34212(17) 0.47467(13) 0.0654(7) Uani 1 1 d . . . S5 S 0.16361(18) 0.66843(18) 0.07616(12) 0.0667(8) Uani 1 1 d . . . S2 S 0.21248(19) 0.11070(16) 0.27671(13) 0.0653(7) Uani 1 1 d . . . S4 S 0.34304(18) 0.92790(16) 0.24254(13) 0.0655(7) Uani 1 1 d . . . S3 S 0.4548(2) 0.1371(2) 0.57802(14) 0.0838(9) Uani 1 1 d . . . S6 S 0.0557(2) 0.8627(2) -0.05661(14) 0.0823(9) Uani 1 1 d . . . P1 P 0.7633(3) 0.4973(2) 0.7648(2) 0.1024(12) Uani 1 1 d . . . O13 O 0.6845(6) 0.4322(7) 0.7801(7) 0.245(7) Uani 1 1 d . . . O16 O 0.7163(6) 0.5399(4) 0.7002(4) 0.144(4) Uani 1 1 d . . . O14 O 0.8281(6) 0.5697(6) 0.8366(4) 0.123(3) Uani 1 1 d . . . O15 O 0.8400(9) 0.4426(6) 0.7499(5) 0.181(5) Uani 1 1 d . . . N1 N 0.5207(6) 0.2509(5) 0.3901(4) 0.0543(19) Uani 1 1 d D . . C1 C 0.6215(7) 0.3123(7) 0.4514(5) 0.082(3) Uani 1 1 d . . . H1A H 0.6747 0.3210 0.4307 0.099 Uiso 1 1 calc R . . H1B H 0.6438 0.2820 0.4917 0.099 Uiso 1 1 calc R . . C2 C 0.6066(7) 0.4118(6) 0.4846(5) 0.061(3) Uani 1 1 d . . . H2A H 0.6694 0.4597 0.4962 0.074 Uiso 1 1 calc R . . H2B H 0.5507 0.4250 0.4462 0.074 Uiso 1 1 calc R . . N2 N 0.5841(6) 0.4170(5) 0.5511(4) 0.069(2) Uani 1 1 d . . . H2N H 0.6355 0.4375 0.5940 0.082 Uiso 1 1 calc R . . N3 N 0.4915(6) 0.4182(5) 0.6244(4) 0.067(2) Uani 1 1 d . . . H3N H 0.5505 0.4525 0.6571 0.081 Uiso 1 1 calc R . . C3 C 0.4872(7) 0.3917(6) 0.5517(6) 0.060(3) Uani 1 1 d . . . C10 C 0.5019(7) 0.2825(6) 0.3174(5) 0.065(3) Uani 1 1 d . . . H10A H 0.5503 0.2651 0.2958 0.079 Uiso 1 1 calc R . . H10B H 0.5159 0.3500 0.3299 0.079 Uiso 1 1 calc R . . C11 C 0.3915(7) 0.2406(7) 0.2581(5) 0.075(3) Uani 1 1 d . . . H11A H 0.3896 0.2537 0.2108 0.090 Uiso 1 1 calc R . . H11B H 0.3753 0.1733 0.2499 0.090 Uiso 1 1 calc R . . N6 N 0.1730(6) 0.2779(5) 0.3004(4) 0.059(2) Uani 1 1 d . . . H6N H 0.1924 0.3361 0.3027 0.071 Uiso 1 1 calc R . . N5 N 0.3119(6) 0.2742(5) 0.2771(3) 0.056(2) Uani 1 1 d . . . H5N H 0.3175 0.3332 0.2844 0.068 Uiso 1 1 calc R . . C12 C 0.2319(7) 0.2242(7) 0.2844(4) 0.052(2) Uani 1 1 d . . . C18 C 0.0057(8) 0.1685(7) 0.2756(5) 0.064(3) Uani 1 1 d . . . H18 H 0.0126 0.1263 0.2375 0.077 Uiso 1 1 calc R . . C13 C 0.0834(8) 0.2501(7) 0.3139(5) 0.061(3) Uani 1 1 d . . . C14 C 0.0679(8) 0.3117(7) 0.3719(6) 0.078(3) Uani 1 1 d . . . H14 H 0.1182 0.3675 0.3990 0.094 Uiso 1 1 calc R . . C15 C -0.0204(9) 0.2912(9) 0.3896(6) 0.087(3) Uani 1 1 d . . . H15 H -0.0310 0.3311 0.4271 0.105 Uiso 1 1 calc R . . C16 C -0.0898(8) 0.2066(9) 0.3464(6) 0.067(3) Uani 1 1 d . . . C17 C -0.0806(7) 0.1478(7) 0.2916(5) 0.065(3) Uani 1 1 d . . . H17 H -0.1323 0.0929 0.2642 0.078 Uiso 1 1 calc R . . N7 N -0.1806(9) 0.1853(9) 0.3665(7) 0.100(3) Uani 1 1 d . . . O4 O -0.2471(7) 0.1129(7) 0.3293(5) 0.116(3) Uani 1 1 d . . . O3 O -0.1855(7) 0.2383(8) 0.4204(6) 0.152(4) Uani 1 1 d . . . C19 C 0.5303(7) 0.1525(6) 0.3772(5) 0.062(3) Uani 1 1 d . . . H19A H 0.5989 0.1520 0.3782 0.075 Uiso 1 1 calc R . . H19B H 0.4801 0.1160 0.3278 0.075 Uiso 1 1 calc R . . C20 C 0.5123(7) 0.1083(7) 0.4376(5) 0.076(3) Uani 1 1 d . . . H20A H 0.5307 0.0492 0.4333 0.091 Uiso 1 1 calc R . . H20B H 0.5570 0.1489 0.4872 0.091 Uiso 1 1 calc R . . N8 N 0.4056(6) 0.0926(5) 0.4310(4) 0.065(2) Uani 1 1 d . . . H8N H 0.3588 0.0719 0.3860 0.078 Uiso 1 1 calc R . . N9 N 0.2676(6) 0.0965(5) 0.4640(4) 0.065(2) Uani 1 1 d . . . H9N H 0.2361 0.0875 0.4160 0.078 Uiso 1 1 calc R . . C21 C 0.3714(8) 0.1070(6) 0.4885(5) 0.061(3) Uani 1 1 d . . . C27 C 0.1206(8) 0.1327(7) 0.4806(5) 0.075(3) Uani 1 1 d . . . H27 H 0.1087 0.1563 0.4384 0.089 Uiso 1 1 calc R . . C25 C 0.0685(9) 0.0962(8) 0.5774(6) 0.077(3) Uani 1 1 d . . . C23 C 0.2204(8) 0.0593(7) 0.5675(5) 0.088(3) Uani 1 1 d . . . H23 H 0.2765 0.0342 0.5851 0.106 Uiso 1 1 calc R . . C22 C 0.2060(8) 0.0982(6) 0.5050(5) 0.061(3) Uani 1 1 d . . . C24 C 0.1474(9) 0.0591(8) 0.6030(6) 0.087(3) Uani 1 1 d . . . H24 H 0.1551 0.0332 0.6437 0.104 Uiso 1 1 calc R . . C26 C 0.0529(8) 0.1332(7) 0.5163(6) 0.082(3) Uani 1 1 d . . . H26 H -0.0033 0.1584 0.4993 0.098 Uiso 1 1 calc R . . N10 N -0.0025(9) 0.0946(8) 0.6184(6) 0.095(3) Uani 1 1 d . . . O5 O 0.0114(7) 0.0623(7) 0.6707(5) 0.131(4) Uani 1 1 d . . . O6 O -0.0743(7) 0.1291(7) 0.5930(5) 0.123(3) Uani 1 1 d . . . N11 N 0.0405(5) 0.7789(5) 0.1620(4) 0.0514(19) Uani 1 1 d D . . C28 C 0.0789(7) 0.7559(7) 0.2411(4) 0.065(3) Uani 1 1 d . . . H28A H 0.0344 0.7721 0.2670 0.078 Uiso 1 1 calc R . . H28B H 0.0712 0.6892 0.2327 0.078 Uiso 1 1 calc R . . C29 C 0.1889(7) 0.8056(6) 0.2913(5) 0.062(3) Uani 1 1 d . . . H29A H 0.2001 0.8715 0.2930 0.074 Uiso 1 1 calc R . . H29B H 0.2010 0.8000 0.3422 0.074 Uiso 1 1 calc R . . N13 N 0.3943(6) 0.7637(6) 0.2278(4) 0.052(2) Uani 1 1 d . . . N12 N 0.2622(6) 0.7692(5) 0.2663(4) 0.062(2) Uani 1 1 d . . . H12N H 0.2594 0.7113 0.2642 0.074 Uiso 1 1 calc R . . C30 C 0.3347(7) 0.8146(6) 0.2457(4) 0.052(2) Uani 1 1 d . . . C36 C 0.5459(7) 0.8754(7) 0.2378(5) 0.057(2) Uani 1 1 d . . . H36 H 0.5371 0.9195 0.2736 0.069 Uiso 1 1 calc R . . C31 C 0.4774(7) 0.7895(7) 0.2058(5) 0.049(2) Uani 1 1 d . . . C35 C 0.6280(7) 0.8961(7) 0.2164(5) 0.066(3) Uani 1 1 d . . . H35 H 0.6749 0.9547 0.2378 0.079 Uiso 1 1 calc R . . C32 C 0.4896(8) 0.7234(7) 0.1542(6) 0.072(3) Uani 1 1 d . . . H32 H 0.4430 0.6646 0.1329 0.086 Uiso 1 1 calc R . . C34 C 0.6415(8) 0.8322(9) 0.1647(6) 0.068(3) Uani 1 1 d . . . C33 C 0.5741(10) 0.7470(8) 0.1346(6) 0.087(3) Uani 1 1 d . . . H33 H 0.5846 0.7028 0.0997 0.105 Uiso 1 1 calc R . . N14 N 0.7309(8) 0.8515(9) 0.1401(7) 0.095(3) Uani 1 1 d . . . O8 O 0.7940(7) 0.9280(7) 0.1745(5) 0.115(3) Uani 1 1 d . . . O7 O 0.7365(8) 0.7951(8) 0.0899(6) 0.157(4) Uani 1 1 d . . . N16 N 0.0440(5) 0.6095(4) -0.0726(4) 0.0506(19) Uani 1 1 d . . . H16N H -0.0182 0.5848 -0.1053 0.061 Uiso 1 1 calc R . . N15 N -0.0378(6) 0.6079(5) 0.0059(4) 0.060(2) Uani 1 1 d . . . H15N H -0.0924 0.5904 -0.0351 0.072 Uiso 1 1 calc R . . C37 C -0.0645(6) 0.7119(6) 0.1095(5) 0.062(3) Uani 1 1 d . . . H37A H -0.0977 0.7389 0.0692 0.075 Uiso 1 1 calc R . . H37B H -0.1086 0.7038 0.1378 0.075 Uiso 1 1 calc R . . C38 C -0.0532(7) 0.6146(6) 0.0746(5) 0.070(3) Uani 1 1 d . . . H38A H 0.0050 0.6012 0.1110 0.084 Uiso 1 1 calc R . . H38B H -0.1150 0.5673 0.0658 0.084 Uiso 1 1 calc R . . C39 C 0.0522(7) 0.6260(6) -0.0009(5) 0.048(2) Uani 1 1 d . . . C40 C 0.1179(8) 0.6250(6) -0.1037(5) 0.058(3) Uani 1 1 d . . . C42 C 0.2869(7) 0.6452(7) -0.1074(6) 0.079(3) Uani 1 1 d . . . H42 H 0.3578 0.6526 -0.0841 0.095 Uiso 1 1 calc R . . C41 C 0.2225(8) 0.6293(6) -0.0683(5) 0.071(3) Uani 1 1 d . . . H41 H 0.2486 0.6218 -0.0196 0.085 Uiso 1 1 calc R . . C43 C 0.2438(11) 0.6498(7) -0.1812(7) 0.082(3) Uani 1 1 d . . . C45 C 0.0849(8) 0.6304(8) -0.1773(6) 0.091(4) Uani 1 1 d . . . H45 H 0.0148 0.6255 -0.2019 0.109 Uiso 1 1 calc R . . C44 C 0.1432(9) 0.6417(9) -0.2154(7) 0.101(4) Uani 1 1 d . . . H44 H 0.1154 0.6442 -0.2654 0.121 Uiso 1 1 calc R . . N17 N 0.3145(9) 0.6649(8) -0.2228(7) 0.115(4) Uani 1 1 d . . . O10 O 0.4090(7) 0.6722(5) -0.1866(5) 0.112(3) Uani 1 1 d . . . O9 O 0.2823(9) 0.6755(10) -0.2842(6) 0.220(7) Uani 1 1 d . . . N18 N 0.1335(6) 0.9137(5) 0.0928(4) 0.068(2) Uani 1 1 d . . . H18N H 0.1868 0.9324 0.1346 0.082 Uiso 1 1 calc R . . N19 N 0.2539(6) 0.9025(5) 0.0441(4) 0.072(2) Uani 1 1 d . . . H19N H 0.2926 0.9160 0.0913 0.086 Uiso 1 1 calc R . . N20 N 0.4977(10) 0.8878(7) -0.1315(6) 0.095(3) Uani 1 1 d . . . O11 O 0.4628(7) 0.8972(6) -0.1955(5) 0.122(3) Uani 1 1 d . . . O12 O 0.5846(7) 0.8804(7) -0.1011(5) 0.130(4) Uani 1 1 d . . . C46 C 0.0336(7) 0.8786(6) 0.1665(5) 0.060(3) Uani 1 1 d . . . H46A H -0.0296 0.8850 0.1734 0.072 Uiso 1 1 calc R . . H46B H 0.0916 0.9199 0.2103 0.072 Uiso 1 1 calc R . . C47 C 0.0344(7) 0.9077(6) 0.0981(5) 0.068(3) Uani 1 1 d . . . H47A H -0.0188 0.8628 0.0536 0.082 Uiso 1 1 calc R . . H47B H 0.0189 0.9680 0.1000 0.082 Uiso 1 1 calc R . . C52 C 0.4322(9) 0.8871(7) -0.0886(6) 0.070(3) Uani 1 1 d . . . C49 C 0.3091(8) 0.8938(6) -0.0048(5) 0.063(3) Uani 1 1 d . . . C51 C 0.3380(10) 0.9041(7) -0.1188(6) 0.083(3) Uani 1 1 d . . . H51 H 0.3153 0.9137 -0.1669 0.099 Uiso 1 1 calc R . . C53 C 0.4657(8) 0.8766(7) -0.0166(6) 0.077(3) Uani 1 1 d . . . H53 H 0.5311 0.8671 0.0046 0.092 Uiso 1 1 calc R . . C54 C 0.4052(8) 0.8799(7) 0.0244(6) 0.075(3) Uani 1 1 d . . . H54 H 0.4298 0.8726 0.0732 0.090 Uiso 1 1 calc R . . C48 C 0.1512(8) 0.8933(6) 0.0299(5) 0.056(2) Uani 1 1 d . . . C50 C 0.2766(8) 0.9070(7) -0.0772(6) 0.087(3) Uani 1 1 d . . . H50 H 0.2118 0.9179 -0.0981 0.104 Uiso 1 1 calc R . . O17 O 0.9085(6) 0.4068(6) 0.6059(4) 0.131(3) Uani 1 1 d . . . H13N H 0.385(6) 0.705(5) 0.213(4) 0.05(3) Uiso 1 1 d . . . C4 C 0.4163(8) 0.3986(7) 0.6528(6) 0.061(3) Uani 1 1 d . . . C7 C 0.2773(11) 0.3658(8) 0.7201(8) 0.101(4) Uani 1 1 d . . . C8 C 0.3630(12) 0.4343(10) 0.7564(6) 0.109(4) Uani 1 1 d . . . H8 H 0.3752 0.4719 0.8036 0.131 Uiso 1 1 calc R . . C6 C 0.2656(12) 0.3136(10) 0.6566(7) 0.172(8) Uani 1 1 d . . . H6 H 0.2078 0.2628 0.6322 0.207 Uiso 1 1 calc R . . C9 C 0.4359(8) 0.4496(8) 0.7223(6) 0.096(4) Uani 1 1 d . . . H9 H 0.4980 0.4955 0.7484 0.115 Uiso 1 1 calc R . . C5 C 0.3363(11) 0.3304(10) 0.6234(8) 0.156(7) Uani 1 1 d . . . H5 H 0.3247 0.2901 0.5774 0.187 Uiso 1 1 calc R . . N4 N 0.2047(10) 0.3425(11) 0.7586(7) 0.128(4) Uani 1 1 d . . . O1 O 0.1420(10) 0.2763(11) 0.7349(8) 0.304(12) Uani 1 1 d . . . O2 O 0.2109(9) 0.4032(7) 0.8098(7) 0.197(6) Uani 1 1 d . . . O18 O 0.6090(10) 0.5458(9) 0.9810(7) 0.249(6) Uiso 1 1 d . . . O19 O 0.7967(10) 0.7889(9) 0.9288(7) 0.252(6) Uiso 1 1 d . . . H11N H 0.078(6) 0.753(6) 0.138(4) 0.10(4) Uiso 1 1 d D . . H1N H 0.464(4) 0.261(7) 0.399(5) 0.11(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0552(16) 0.0612(17) 0.0714(16) 0.0008(14) 0.0218(14) 0.0169(14) S5 0.0492(15) 0.090(2) 0.0518(14) 0.0058(14) 0.0146(12) 0.0176(14) S2 0.0722(18) 0.0450(16) 0.0756(17) 0.0139(13) 0.0249(14) 0.0165(14) S4 0.0645(17) 0.0494(16) 0.0751(17) 0.0153(13) 0.0179(14) 0.0156(13) S3 0.079(2) 0.113(2) 0.0624(17) 0.0300(16) 0.0192(15) 0.0394(18) S6 0.078(2) 0.105(2) 0.0630(16) 0.0245(16) 0.0231(15) 0.0248(17) P1 0.071(2) 0.077(2) 0.133(3) 0.061(2) -0.002(2) 0.005(2) O13 0.075(6) 0.185(10) 0.447(19) 0.242(12) -0.002(8) 0.002(6) O16 0.166(8) 0.042(4) 0.131(6) 0.028(4) -0.050(6) 0.006(5) O14 0.111(6) 0.117(7) 0.099(6) 0.031(5) -0.009(5) 0.020(5) O15 0.286(13) 0.124(8) 0.155(8) 0.057(7) 0.063(8) 0.129(9) N1 0.052(5) 0.054(5) 0.059(5) 0.007(4) 0.029(4) 0.010(4) C1 0.049(7) 0.104(9) 0.079(7) 0.001(7) 0.029(6) 0.000(6) C2 0.072(7) 0.044(6) 0.067(6) 0.003(5) 0.038(5) 0.001(5) N2 0.078(6) 0.069(6) 0.060(5) 0.015(4) 0.031(5) 0.015(5) N3 0.061(5) 0.083(6) 0.048(5) -0.001(4) 0.026(4) 0.001(5) C3 0.060(7) 0.028(5) 0.100(8) 0.013(5) 0.042(7) 0.012(5) C10 0.057(7) 0.080(7) 0.068(6) 0.022(6) 0.038(6) 0.011(6) C11 0.078(8) 0.097(8) 0.057(6) 0.029(6) 0.028(6) 0.029(7) N6 0.053(5) 0.054(5) 0.088(6) 0.027(4) 0.041(5) 0.017(4) N5 0.063(5) 0.053(5) 0.063(5) 0.013(4) 0.029(4) 0.031(5) C12 0.038(6) 0.069(8) 0.049(5) 0.015(5) 0.019(5) 0.009(5) C18 0.075(8) 0.059(7) 0.048(6) 0.002(5) 0.014(6) 0.022(6) C13 0.075(8) 0.055(7) 0.049(6) 0.013(5) 0.009(6) 0.037(6) C14 0.074(8) 0.062(7) 0.084(8) 0.011(6) 0.015(6) 0.023(6) C15 0.074(8) 0.119(11) 0.091(8) 0.027(8) 0.051(8) 0.040(8) C16 0.045(7) 0.094(9) 0.076(8) 0.040(7) 0.031(6) 0.020(7) C17 0.051(7) 0.081(8) 0.059(6) 0.004(6) 0.032(6) 0.004(6) N7 0.087(9) 0.123(11) 0.111(10) 0.042(9) 0.045(8) 0.053(8) O4 0.081(7) 0.140(9) 0.138(8) 0.032(7) 0.060(6) 0.020(6) O3 0.115(7) 0.193(11) 0.169(9) 0.013(8) 0.100(7) 0.041(7) C19 0.072(7) 0.039(6) 0.093(7) 0.018(5) 0.045(6) 0.025(5) C20 0.067(7) 0.079(8) 0.092(8) 0.019(6) 0.035(6) 0.039(6) N8 0.062(6) 0.053(5) 0.069(5) 0.007(4) 0.023(5) 0.006(4) N9 0.051(5) 0.099(7) 0.054(5) 0.029(4) 0.027(4) 0.021(5) C21 0.090(8) 0.054(6) 0.062(6) 0.022(5) 0.049(6) 0.023(6) C27 0.065(7) 0.106(9) 0.066(6) 0.049(6) 0.025(6) 0.032(7) C25 0.069(8) 0.096(9) 0.074(8) 0.021(7) 0.035(7) 0.024(7) C23 0.102(9) 0.106(9) 0.078(7) 0.052(7) 0.032(7) 0.052(7) C22 0.064(7) 0.067(7) 0.047(6) 0.019(5) 0.017(5) 0.007(6) C24 0.091(9) 0.116(10) 0.083(8) 0.043(7) 0.059(8) 0.031(8) C26 0.076(8) 0.106(9) 0.075(7) 0.035(7) 0.034(7) 0.026(7) N10 0.092(9) 0.111(9) 0.093(8) 0.015(7) 0.056(8) 0.026(7) O5 0.161(8) 0.167(9) 0.085(6) 0.043(6) 0.077(6) 0.025(7) O6 0.116(8) 0.155(9) 0.118(7) 0.021(6) 0.076(6) 0.037(7) N11 0.048(5) 0.060(6) 0.054(5) 0.017(4) 0.029(4) 0.013(4) C28 0.070(7) 0.094(8) 0.061(6) 0.033(6) 0.047(6) 0.033(6) C29 0.055(6) 0.081(7) 0.056(6) 0.021(5) 0.026(5) 0.022(6) N13 0.068(6) 0.031(5) 0.062(5) 0.008(4) 0.027(4) 0.025(5) N12 0.060(5) 0.066(6) 0.076(5) 0.035(4) 0.033(5) 0.027(5) C30 0.055(6) 0.048(6) 0.043(5) 0.014(5) 0.011(5) 0.005(5) C36 0.055(6) 0.069(8) 0.053(6) 0.011(5) 0.032(5) 0.011(6) C31 0.040(6) 0.061(7) 0.055(6) 0.023(5) 0.024(5) 0.014(5) C35 0.065(7) 0.068(7) 0.058(6) 0.010(6) 0.019(6) 0.015(6) C32 0.076(8) 0.066(8) 0.095(8) 0.014(6) 0.053(7) 0.036(6) C34 0.057(7) 0.078(9) 0.091(8) 0.038(7) 0.041(7) 0.028(7) C33 0.098(10) 0.081(9) 0.091(8) 0.001(7) 0.046(8) 0.045(8) N14 0.072(8) 0.110(10) 0.113(9) 0.043(8) 0.039(8) 0.029(7) O8 0.094(7) 0.149(9) 0.131(8) 0.061(7) 0.062(6) 0.038(6) O7 0.162(9) 0.166(10) 0.183(10) 0.011(8) 0.126(9) 0.052(8) N16 0.036(4) 0.059(5) 0.052(5) 0.008(4) 0.018(4) 0.006(4) N15 0.058(5) 0.072(6) 0.042(4) 0.000(4) 0.022(4) 0.006(4) C37 0.041(6) 0.082(8) 0.061(6) 0.013(5) 0.022(5) 0.007(5) C38 0.056(6) 0.044(6) 0.097(8) 0.003(6) 0.032(6) -0.008(5) C39 0.052(6) 0.045(6) 0.061(6) 0.020(5) 0.033(5) 0.016(5) C40 0.059(7) 0.038(6) 0.069(7) 0.013(5) 0.014(6) 0.013(5) C42 0.055(7) 0.079(8) 0.100(9) 0.014(7) 0.032(7) 0.017(6) C41 0.073(8) 0.092(8) 0.065(6) 0.018(6) 0.045(6) 0.027(6) C43 0.111(11) 0.076(8) 0.089(9) 0.037(7) 0.073(9) 0.010(7) C45 0.058(7) 0.150(11) 0.076(8) 0.069(8) 0.026(6) 0.016(7) C44 0.059(8) 0.155(12) 0.099(9) 0.063(8) 0.025(8) 0.036(8) N17 0.079(8) 0.131(10) 0.129(10) 0.047(8) 0.034(9) 0.009(8) O10 0.123(7) 0.105(7) 0.134(7) 0.031(6) 0.088(7) 0.018(6) O9 0.169(10) 0.43(2) 0.146(9) 0.185(12) 0.100(8) 0.105(11) N18 0.066(6) 0.090(6) 0.060(5) 0.042(5) 0.028(5) 0.017(5) N19 0.067(6) 0.098(7) 0.062(5) 0.038(5) 0.033(5) 0.017(5) N20 0.120(10) 0.074(7) 0.097(9) 0.006(6) 0.063(9) 0.013(7) O11 0.157(8) 0.159(8) 0.103(6) 0.055(6) 0.090(6) 0.067(7) O12 0.091(7) 0.174(9) 0.113(7) -0.011(6) 0.053(6) 0.028(7) C46 0.072(7) 0.051(6) 0.078(7) 0.014(5) 0.046(6) 0.033(5) C47 0.086(8) 0.072(7) 0.079(7) 0.041(6) 0.051(6) 0.042(6) C52 0.077(8) 0.064(7) 0.090(8) 0.028(6) 0.050(8) 0.027(6) C49 0.085(8) 0.050(6) 0.053(6) 0.024(5) 0.022(6) 0.013(6) C51 0.111(10) 0.096(9) 0.080(7) 0.048(7) 0.066(8) 0.036(8) C53 0.076(8) 0.090(8) 0.078(8) 0.023(7) 0.036(7) 0.039(7) C54 0.064(7) 0.098(9) 0.071(7) 0.033(6) 0.022(6) 0.039(7) C48 0.073(7) 0.048(6) 0.051(6) 0.022(5) 0.021(6) 0.017(5) C50 0.071(8) 0.110(10) 0.090(8) 0.046(7) 0.025(7) 0.039(7) O17 0.166(8) 0.145(8) 0.079(5) 0.042(5) 0.047(5) 0.020(6) C4 0.062(7) 0.054(7) 0.068(7) 0.004(6) 0.035(6) 0.014(6) C7 0.119(11) 0.047(8) 0.131(12) -0.003(7) 0.077(10) -0.021(7) C8 0.169(14) 0.123(12) 0.067(8) 0.032(8) 0.069(10) 0.061(11) C6 0.178(15) 0.161(14) 0.115(11) -0.070(10) 0.101(11) -0.090(11) C9 0.087(9) 0.128(11) 0.067(7) 0.012(7) 0.038(7) 0.010(8) C5 0.139(12) 0.139(12) 0.145(12) -0.068(10) 0.109(11) -0.073(10) N4 0.104(9) 0.184(14) 0.127(10) 0.015(10) 0.091(9) 0.049(10) O1 0.180(12) 0.323(18) 0.277(15) -0.159(13) 0.174(12) -0.180(12) O2 0.269(14) 0.107(8) 0.296(14) 0.006(8) 0.254(13) 0.007(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C3 1.625(10) . ? S5 C39 1.688(9) . ? S2 C12 1.654(9) . ? S4 C30 1.705(9) . ? S3 C21 1.666(9) . ? S6 C48 1.685(9) . ? P1 O14 1.486(8) . ? P1 O13 1.499(9) . ? P1 O16 1.525(7) . ? P1 O15 1.549(10) . ? N1 C19 1.498(10) . ? N1 C1 1.516(10) . ? N1 C10 1.528(10) . ? C1 C2 1.602(11) . ? C2 N2 1.428(9) . ? N2 C3 1.367(10) . ? N3 C4 1.372(10) . ? N3 C3 1.377(10) . ? C10 C11 1.532(11) . ? C11 N5 1.447(10) . ? N6 C12 1.335(10) . ? N6 C13 1.393(11) . ? N5 C12 1.312(9) . ? C18 C17 1.363(11) . ? C18 C13 1.383(12) . ? C13 C14 1.430(12) . ? C14 C15 1.408(12) . ? C15 C16 1.380(13) . ? C16 C17 1.316(12) . ? C16 N7 1.471(14) . ? N7 O4 1.221(11) . ? N7 O3 1.227(11) . ? C19 C20 1.525(11) . ? C20 N8 1.449(10) . ? N8 C21 1.361(10) . ? N9 C21 1.356(10) . ? N9 C22 1.371(10) . ? C27 C26 1.365(11) . ? C27 C22 1.375(11) . ? C25 C24 1.328(12) . ? C25 C26 1.374(13) . ? C25 N10 1.483(13) . ? C23 C22 1.416(11) . ? C23 C24 1.428(12) . ? N10 O5 1.182(11) . ? N10 O6 1.224(11) . ? N11 C46 1.512(10) . ? N11 C37 1.531(10) . ? N11 C28 1.577(9) . ? C28 C29 1.497(10) . ? C29 N12 1.439(9) . ? N13 C30 1.327(10) . ? N13 C31 1.402(10) . ? N12 C30 1.349(10) . ? C36 C31 1.363(11) . ? C36 C35 1.370(11) . ? C31 C32 1.359(11) . ? C35 C34 1.350(12) . ? C32 C33 1.388(13) . ? C34 C33 1.349(13) . ? C34 N14 1.503(13) . ? N14 O7 1.208(11) . ? N14 O8 1.235(11) . ? N16 C39 1.334(9) . ? N16 C40 1.385(10) . ? N15 C39 1.316(9) . ? N15 C38 1.416(10) . ? C37 C38 1.561(11) . ? C40 C45 1.373(11) . ? C40 C41 1.394(11) . ? C42 C43 1.380(13) . ? C42 C41 1.391(11) . ? C43 C44 1.329(13) . ? C43 N17 1.501(14) . ? C45 C44 1.296(12) . ? N17 O9 1.180(12) . ? N17 O10 1.261(11) . ? N18 C48 1.325(10) . ? N18 C47 1.435(10) . ? N19 C48 1.366(10) . ? N19 C49 1.428(11) . ? N20 O12 1.211(11) . ? N20 O11 1.222(11) . ? N20 C52 1.446(13) . ? C46 C47 1.481(10) . ? C52 C51 1.359(12) . ? C52 C53 1.370(12) . ? C49 C54 1.360(11) . ? C49 C50 1.392(12) . ? C51 C50 1.379(12) . ? C53 C54 1.359(11) . ? C4 C5 1.266(12) . ? C4 C9 1.338(12) . ? C7 C6 1.280(14) . ? C7 C8 1.323(14) . ? C7 N4 1.496(15) . ? C8 C9 1.415(14) . ? C6 C5 1.379(14) . ? N4 O1 1.113(14) . ? N4 O2 1.192(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O14 P1 O13 107.7(7) . . ? O14 P1 O16 112.3(4) . . ? O13 P1 O16 113.7(5) . . ? O14 P1 O15 103.5(5) . . ? O13 P1 O15 107.5(6) . . ? O16 P1 O15 111.6(6) . . ? C19 N1 C1 107.6(7) . . ? C19 N1 C10 110.2(7) . . ? C1 N1 C10 109.7(7) . . ? N1 C1 C2 110.4(7) . . ? N2 C2 C1 113.4(7) . . ? C3 N2 C2 125.0(8) . . ? C4 N3 C3 130.1(8) . . ? N2 C3 N3 109.9(8) . . ? N2 C3 S1 122.1(8) . . ? N3 C3 S1 127.9(7) . . ? N1 C10 C11 113.6(7) . . ? N5 C11 C10 115.2(8) . . ? C12 N6 C13 127.2(8) . . ? C12 N5 C11 126.9(8) . . ? N5 C12 N6 110.7(8) . . ? N5 C12 S2 122.9(8) . . ? N6 C12 S2 126.4(7) . . ? C17 C18 C13 122.4(9) . . ? C18 C13 N6 126.3(9) . . ? C18 C13 C14 115.8(10) . . ? N6 C13 C14 117.9(10) . . ? C15 C14 C13 122.6(10) . . ? C16 C15 C14 114.0(10) . . ? C17 C16 C15 126.2(10) . . ? C17 C16 N7 120.4(11) . . ? C15 C16 N7 113.4(11) . . ? C16 C17 C18 119.0(10) . . ? O4 N7 O3 122.8(13) . . ? O4 N7 C16 117.3(12) . . ? O3 N7 C16 119.8(13) . . ? N1 C19 C20 111.0(7) . . ? N8 C20 C19 112.2(8) . . ? C21 N8 C20 126.9(8) . . ? C21 N9 C22 129.0(8) . . ? N9 C21 N8 113.0(8) . . ? N9 C21 S3 126.6(7) . . ? N8 C21 S3 120.4(8) . . ? C26 C27 C22 122.1(9) . . ? C24 C25 C26 122.2(11) . . ? C24 C25 N10 116.0(11) . . ? C26 C25 N10 121.8(11) . . ? C22 C23 C24 118.9(10) . . ? N9 C22 C27 118.4(8) . . ? N9 C22 C23 123.5(10) . . ? C27 C22 C23 117.9(9) . . ? C25 C24 C23 119.6(10) . . ? C27 C26 C25 119.3(10) . . ? O5 N10 O6 124.6(12) . . ? O5 N10 C25 121.4(12) . . ? O6 N10 C25 114.0(11) . . ? C46 N11 C37 109.5(7) . . ? C46 N11 C28 114.1(7) . . ? C37 N11 C28 110.5(6) . . ? C29 C28 N11 114.6(7) . . ? N12 C29 C28 112.6(7) . . ? C30 N13 C31 129.4(9) . . ? C30 N12 C29 128.2(8) . . ? N13 C30 N12 114.8(8) . . ? N13 C30 S4 125.0(8) . . ? N12 C30 S4 120.2(8) . . ? C31 C36 C35 119.2(9) . . ? C32 C31 C36 121.5(9) . . ? C32 C31 N13 117.0(9) . . ? C36 C31 N13 121.4(9) . . ? C34 C35 C36 120.6(10) . . ? C31 C32 C33 117.4(10) . . ? C33 C34 C35 119.5(10) . . ? C33 C34 N14 118.0(12) . . ? C35 C34 N14 122.5(11) . . ? C34 C33 C32 121.7(10) . . ? O7 N14 O8 125.1(13) . . ? O7 N14 C34 120.5(12) . . ? O8 N14 C34 114.4(12) . . ? C39 N16 C40 131.4(7) . . ? C39 N15 C38 126.0(7) . . ? N11 C37 C38 111.8(7) . . ? N15 C38 C37 114.2(7) . . ? N15 C39 N16 113.3(7) . . ? N15 C39 S5 120.8(7) . . ? N16 C39 S5 125.8(7) . . ? C45 C40 N16 117.7(9) . . ? C45 C40 C41 116.7(10) . . ? N16 C40 C41 125.4(9) . . ? C43 C42 C41 118.9(10) . . ? C42 C41 C40 118.5(9) . . ? C44 C43 C42 122.0(10) . . ? C44 C43 N17 120.0(12) . . ? C42 C43 N17 118.0(12) . . ? C44 C45 C40 125.5(11) . . ? C45 C44 C43 118.3(11) . . ? O9 N17 O10 123.1(13) . . ? O9 N17 C43 120.3(12) . . ? O10 N17 C43 116.4(11) . . ? C48 N18 C47 126.6(8) . . ? C48 N19 C49 132.0(8) . . ? O12 N20 O11 124.0(12) . . ? O12 N20 C52 117.6(12) . . ? O11 N20 C52 118.3(12) . . ? C47 C46 N11 112.6(7) . . ? N18 C47 C46 110.7(7) . . ? C51 C52 C53 119.4(10) . . ? C51 C52 N20 118.7(11) . . ? C53 C52 N20 121.7(11) . . ? C54 C49 C50 117.6(10) . . ? C54 C49 N19 117.0(8) . . ? C50 C49 N19 125.2(10) . . ? C52 C51 C50 119.1(10) . . ? C54 C53 C52 121.3(10) . . ? C53 C54 C49 120.9(10) . . ? N18 C48 N19 112.3(8) . . ? N18 C48 S6 122.4(8) . . ? N19 C48 S6 125.3(7) . . ? C51 C50 C49 121.6(10) . . ? C5 C4 C9 116.9(11) . . ? C5 C4 N3 126.1(10) . . ? C9 C4 N3 116.4(10) . . ? C6 C7 C8 118.4(13) . . ? C6 C7 N4 121.3(13) . . ? C8 C7 N4 119.7(13) . . ? C7 C8 C9 119.1(11) . . ? C7 C6 C5 121.8(12) . . ? C4 C9 C8 120.5(11) . . ? C4 C5 C6 122.7(11) . . ? O1 N4 O2 122.8(13) . . ? O1 N4 C7 120.9(14) . . ? O2 N4 C7 115.7(14) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.157 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.133 data_phosphate _database_code_depnum_ccdc_archive 'CCDC 873076' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C27 H30 N10 O6 S3), 3(C8 H20 N), O4 P' _chemical_formula_sum 'C78 H120 N23 O16 P S6' _chemical_formula_weight 1859.36 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' P P 0.1023 0.0942 '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 Trigonal _symmetry_space_group_name_H-M P3(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, z+1/2' '-x, -x+y, z+1/2' 'x-y, -y, z+1/2' _cell_length_a 19.957(3) _cell_length_b 19.957(3) _cell_length_c 14.7921(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5102.1(12) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9927 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 21.73 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.913 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details SADABS _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 omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57085 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 24.78 _reflns_number_total 2865 _reflns_number_gt 2633 _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 'Mercury 2.3' _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. Appropriate bond restraints have been applied in SHELXL-97 to ensure standard bond geometry of a receptor molecule and tetraethylammonium cation which has been refined isotropically due to disorder. The structure Contains Solvent Accessible VOIDS of 568 A3 and no residual electron density was found within them. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0010P] 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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.015(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(12) _refine_ls_number_reflns 2865 _refine_ls_number_parameters 321 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0958 _refine_ls_R_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.2391 _refine_ls_wR_factor_gt 0.2144 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.019 _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 C13 C 0.41042(18) 0.1563(2) -0.0169(3) 0.0659(11) Uani 1 1 d G . . C14 C 0.42232(19) 0.17935(19) -0.1069(3) 0.0802(14) Uani 1 1 d G . . H14 H 0.4682 0.2230 -0.1243 0.096 Uiso 1 1 calc R . . C15 C 0.3657(3) 0.1372(3) -0.1710(3) 0.106(2) Uani 1 1 d G . . H15 H 0.3737 0.1527 -0.2312 0.127 Uiso 1 1 calc R . . C16 C 0.2971(2) 0.0720(3) -0.1451(4) 0.110(3) Uani 1 1 d G . . C17 C 0.28524(18) 0.0489(2) -0.0550(4) 0.109(2) Uani 1 1 d G . . H17 H 0.2394 0.0053 -0.0377 0.131 Uiso 1 1 calc R . . C18 C 0.3419(2) 0.0910(2) 0.0090(4) 0.099(2) Uani 1 1 d G . . H18 H 0.3339 0.0756 0.0692 0.119 Uiso 1 1 calc R . . S1 S 0.06614(8) 0.60807(9) 0.2167(3) 0.0766(4) Uani 1 1 d . . . O1 O -0.1547(4) 0.2872(3) 0.5027(5) 0.143(2) Uani 1 1 d . . . O2 O -0.0996(4) 0.3383(4) 0.6247(6) 0.138(2) Uani 1 1 d . . . N1 N 0.3333 0.6667 0.1230(5) 0.0586(15) Uani 1 3 d S . . N2 N 0.2156(2) 0.6639(2) 0.2500(3) 0.0584(9) Uani 1 1 d . . . H2 H 0.2514 0.6665 0.2848 0.070 Uiso 1 1 d R . . N3 N 0.1377(2) 0.5903(2) 0.3619(3) 0.0578(9) Uani 1 1 d . . . H3 H 0.1788 0.6127 0.3945 0.069 Uiso 1 1 d R . . N4 N -0.1028(3) 0.3397(3) 0.5445(6) 0.0956(17) Uani 1 1 d . . . C1 C 0.2637(3) 0.6673(3) 0.0970(4) 0.0693(13) Uani 1 1 d . . . H1A H 0.2218 0.6144 0.0901 0.083 Uiso 1 1 calc R . . H1B H 0.2720 0.6929 0.0390 0.083 Uiso 1 1 calc R . . C2 C 0.2403(3) 0.7086(3) 0.1664(4) 0.0664(12) Uani 1 1 d . . . H2A H 0.2838 0.7597 0.1786 0.080 Uiso 1 1 calc R . . H2B H 0.1983 0.7146 0.1425 0.080 Uiso 1 1 calc R . . C3 C 0.1431(3) 0.6204(3) 0.2767(4) 0.0559(10) Uani 1 1 d . . . C4 C 0.0738(2) 0.5280(3) 0.4019(4) 0.0540(9) Uani 1 1 d . . . C5 C 0.0189(3) 0.4634(3) 0.3544(4) 0.0645(11) Uani 1 1 d . . . H5 H 0.0216 0.4617 0.2918 0.077 Uiso 1 1 calc R . . C6 C -0.0401(3) 0.4012(3) 0.4013(5) 0.0735(13) Uani 1 1 d . . . H6 H -0.0773 0.3577 0.3706 0.088 Uiso 1 1 calc R . . C7 C -0.0419(3) 0.4056(3) 0.4945(5) 0.0704(13) Uani 1 1 d . . . C8 C 0.0114(3) 0.4677(3) 0.5419(4) 0.0668(12) Uani 1 1 d . . . H8 H 0.0090 0.4687 0.6046 0.080 Uiso 1 1 calc R . . C9 C 0.0687(3) 0.5288(3) 0.4954(4) 0.0590(10) Uani 1 1 d . . . H9 H 0.1050 0.5720 0.5273 0.071 Uiso 1 1 calc R . . S2 S 0.41212(11) 0.13998(14) 0.2049(3) 0.1086(7) Uani 1 1 d . . . O3 O 0.1818(6) -0.0320(6) -0.1859(10) 0.224(5) Uani 1 1 d . . . O4 O 0.2464(6) 0.0441(7) -0.2805(9) 0.198(5) Uani 1 1 d . . . N5 N 0.6667 0.3333 0.2711(6) 0.0717(19) Uani 1 3 d S . . N6 N 0.5561(2) 0.2075(2) 0.1441(4) 0.0645(10) Uani 1 1 d . . . H6N H 0.5894 0.2325 0.1024 0.077 Uiso 1 1 d R . . N7 N 0.4719(2) 0.1997(2) 0.0406(4) 0.0641(10) Uani 1 1 d . . . H7N H 0.5076 0.2431 0.0194 0.077 Uiso 1 1 d R . . N8 N 0.2394(5) 0.0253(5) -0.2073(8) 0.140(3) Uani 1 1 d . . . C10 C 0.5996(4) 0.2588(4) 0.2980(4) 0.0804(15) Uani 1 1 d . . . H10A H 0.5539 0.2641 0.3015 0.097 Uiso 1 1 calc R . . H10B H 0.6087 0.2445 0.3575 0.097 Uiso 1 1 calc R . . C11 C 0.5859(4) 0.1963(3) 0.2313(4) 0.0781(15) Uani 1 1 d . . . H11A H 0.6341 0.1966 0.2208 0.094 Uiso 1 1 calc R . . H11B H 0.5490 0.1463 0.2564 0.094 Uiso 1 1 calc R . . C12 C 0.4840(3) 0.1836(3) 0.1263(4) 0.0643(12) Uani 1 1 d . . . P1 P 0.3333 0.6667 0.4535(3) 0.0426(4) Uani 1 3 d S . . O5 O 0.3333 0.6667 0.3500(4) 0.0493(11) Uani 1 3 d S . . O6 O 0.33957(16) 0.59721(16) 0.4882(3) 0.0503(7) Uani 1 1 d . . . N9 N 0.7342(3) 0.0407(3) 0.4520(4) 0.0825(12) Uiso 1 1 d . . . C22 C 0.6474(7) -0.0647(7) 0.5665(7) 0.144(3) Uiso 1 1 d D . . H22A H 0.6563 -0.0211 0.6026 0.215 Uiso 1 1 calc R . . H22B H 0.6526 -0.1014 0.6035 0.215 Uiso 1 1 calc R . . H22C H 0.5962 -0.0887 0.5415 0.215 Uiso 1 1 calc R . . C19 C 0.7825(13) 0.0622(12) 0.3755(11) 0.226(8) Uiso 1 1 d D . . H19A H 0.8348 0.0792 0.3961 0.271 Uiso 1 1 calc R . . H19B H 0.7829 0.1065 0.3481 0.271 Uiso 1 1 calc R . . C24 C 0.6679(9) 0.1132(8) 0.3922(12) 0.185(5) Uiso 1 1 d D . . H24A H 0.6852 0.1490 0.4419 0.277 Uiso 1 1 calc R . . H24B H 0.6179 0.1034 0.3727 0.277 Uiso 1 1 calc R . . H24C H 0.7039 0.1349 0.3431 0.277 Uiso 1 1 calc R . . C20 C 0.7631(13) 0.0022(12) 0.3028(11) 0.220(8) Uiso 1 1 d D . . H20A H 0.7861 -0.0287 0.3174 0.329 Uiso 1 1 calc R . . H20B H 0.7828 0.0275 0.2458 0.329 Uiso 1 1 calc R . . H20C H 0.7079 -0.0304 0.2988 0.329 Uiso 1 1 calc R . . C21 C 0.7059(10) -0.0380(10) 0.4908(9) 0.202(6) Uiso 1 1 d D . . H21A H 0.7506 -0.0403 0.5126 0.243 Uiso 1 1 calc R . . H21B H 0.6836 -0.0751 0.4419 0.243 Uiso 1 1 calc R . . C25 C 0.7654(10) 0.1027(11) 0.5272(13) 0.204(6) Uiso 1 1 d D . . H25A H 0.7854 0.1552 0.5054 0.245 Uiso 1 1 calc R . . H25B H 0.7300 0.0914 0.5774 0.245 Uiso 1 1 calc R . . C23 C 0.6624(10) 0.0383(8) 0.4221(12) 0.194(6) Uiso 1 1 d D . . H23A H 0.6255 0.0175 0.4714 0.233 Uiso 1 1 calc R . . H23B H 0.6411 0.0019 0.3724 0.233 Uiso 1 1 calc R . . C26 C 0.827(2) 0.081(3) 0.544(4) 0.47(3) Uiso 1 1 d D . . H26A H 0.8107 0.0311 0.5183 0.710 Uiso 1 1 calc R . . H26B H 0.8346 0.0797 0.6078 0.710 Uiso 1 1 calc R . . H26C H 0.8745 0.1188 0.5162 0.710 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 C13 0.055(3) 0.056(3) 0.086(3) -0.001(2) -0.001(2) 0.027(2) C14 0.064(3) 0.080(3) 0.093(4) -0.002(3) -0.009(3) 0.034(3) C15 0.126(6) 0.101(5) 0.095(4) -0.010(4) -0.027(4) 0.059(5) C16 0.068(4) 0.087(5) 0.160(8) -0.027(5) -0.029(4) 0.027(3) C17 0.064(4) 0.095(5) 0.143(7) -0.011(4) -0.011(4) 0.021(3) C18 0.075(4) 0.085(4) 0.130(6) 0.007(4) 0.000(3) 0.035(3) S1 0.0647(8) 0.0991(10) 0.0667(7) 0.0095(6) -0.0132(5) 0.0415(7) O1 0.105(4) 0.092(4) 0.166(6) 0.009(4) 0.023(4) -0.002(3) O2 0.101(4) 0.143(5) 0.127(5) 0.055(4) 0.037(3) 0.029(3) N1 0.068(2) 0.068(2) 0.040(3) 0.000 0.000 0.0340(12) N2 0.057(2) 0.073(2) 0.0519(19) 0.0170(16) 0.0030(15) 0.0369(19) N3 0.0454(17) 0.068(2) 0.0468(18) 0.0052(15) -0.0065(14) 0.0185(16) N4 0.060(3) 0.086(4) 0.124(5) 0.034(3) 0.021(3) 0.023(3) C1 0.079(3) 0.080(3) 0.043(2) 0.008(2) -0.005(2) 0.036(3) C2 0.067(3) 0.069(3) 0.066(3) 0.023(2) 0.007(2) 0.036(2) C3 0.060(3) 0.060(2) 0.049(2) 0.0027(17) -0.0001(18) 0.031(2) C4 0.048(2) 0.061(2) 0.052(2) 0.0015(18) -0.0027(17) 0.0258(19) C5 0.056(2) 0.067(3) 0.058(2) -0.001(2) -0.011(2) 0.021(2) C6 0.052(3) 0.072(3) 0.092(4) -0.004(2) -0.020(2) 0.028(2) C7 0.051(2) 0.069(3) 0.086(4) 0.019(3) 0.012(2) 0.026(2) C8 0.062(3) 0.083(3) 0.061(3) 0.008(2) 0.012(2) 0.040(3) C9 0.053(2) 0.066(3) 0.054(2) -0.0010(19) 0.0004(18) 0.027(2) S2 0.0839(10) 0.1339(15) 0.0951(11) 0.0471(10) 0.0377(8) 0.0448(10) O3 0.126(6) 0.160(8) 0.288(13) -0.040(8) -0.063(7) -0.004(6) O4 0.173(8) 0.216(9) 0.168(8) -0.015(7) -0.088(6) 0.070(7) N5 0.082(3) 0.082(3) 0.051(3) 0.000 0.000 0.0411(15) N6 0.070(3) 0.064(2) 0.052(2) 0.0074(17) 0.0088(17) 0.027(2) N7 0.052(2) 0.059(2) 0.074(2) 0.0078(18) 0.0079(17) 0.0222(18) N8 0.123(6) 0.112(6) 0.152(8) 0.000(5) -0.046(5) 0.034(5) C10 0.094(4) 0.087(4) 0.054(3) 0.014(2) 0.008(2) 0.040(3) C11 0.088(4) 0.087(4) 0.057(3) 0.020(2) 0.007(2) 0.043(3) C12 0.061(3) 0.058(3) 0.069(3) 0.013(2) 0.012(2) 0.027(2) P1 0.0447(6) 0.0447(6) 0.0383(8) 0.000 0.000 0.0223(3) O5 0.0543(17) 0.0543(17) 0.040(2) 0.000 0.000 0.0271(8) O6 0.0574(16) 0.0487(15) 0.0469(14) 0.0028(12) 0.0023(11) 0.0281(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C13 N7 1.385(5) . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 N8 1.403(9) . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? S1 C3 1.682(5) . ? O1 N4 1.211(9) . ? O2 N4 1.190(9) . ? N1 C1 1.447(6) . ? N1 C1 1.447(6) 3_565 ? N1 C1 1.447(6) 2_665 ? N2 C3 1.321(6) . ? N2 C2 1.458(6) . ? N2 H2 0.8600 . ? N3 C3 1.378(6) . ? N3 C4 1.392(6) . ? N3 H3 0.8600 . ? N4 C7 1.467(7) . ? C1 C2 1.529(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C4 C9 1.388(6) . ? C4 C5 1.394(7) . ? C5 C6 1.395(8) . ? C5 H5 0.9300 . ? C6 C7 1.383(9) . ? C6 H6 0.9300 . ? C7 C8 1.356(8) . ? C8 C9 1.369(7) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? S2 C12 1.709(5) . ? O3 N8 1.189(12) . ? O4 N8 1.132(13) . ? N5 C10 1.474(6) 2_655 ? N5 C10 1.474(6) . ? N5 C10 1.474(6) 3_665 ? N6 C12 1.296(7) . ? N6 C11 1.484(7) . ? N6 H6N 0.8603 . ? N7 C12 1.359(7) . ? N7 H7N 0.8598 . ? C10 C11 1.505(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? P1 O5 1.532(5) . ? P1 O6 1.540(3) 3_565 ? P1 O6 1.540(3) 2_665 ? P1 O6 1.540(3) . ? N9 C19 1.407(19) . ? N9 C23 1.478(17) . ? N9 C21 1.492(17) . ? N9 C25 1.546(19) . ? C22 C21 1.5100(10) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C19 C20 1.5096(10) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C24 C23 1.5099(11) . ? C24 H24A 0.9601 . ? C24 H24B 0.9601 . ? C24 H24C 0.9601 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C25 C26 1.5103(16) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C26 H26A 0.9649 . ? C26 H26B 0.9648 . ? C26 H26C 0.9641 . ? 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 N7 C13 C14 115.5(3) . . ? N7 C13 C18 124.5(3) . . ? C14 C13 C18 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 N8 117.4(6) . . ? C15 C16 N8 122.5(6) . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C1 N1 C1 113.2(2) . 3_565 ? C1 N1 C1 113.2(2) . 2_665 ? C1 N1 C1 113.2(2) 3_565 2_665 ? C3 N2 C2 125.3(4) . . ? C3 N2 H2 117.6 . . ? C2 N2 H2 117.0 . . ? C3 N3 C4 128.0(4) . . ? C3 N3 H3 116.1 . . ? C4 N3 H3 115.9 . . ? O2 N4 O1 121.4(6) . . ? O2 N4 C7 119.6(6) . . ? O1 N4 C7 119.0(7) . . ? N1 C1 C2 112.4(4) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C1 109.9(4) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.6 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 N3 112.4(4) . . ? N2 C3 S1 124.0(3) . . ? N3 C3 S1 123.5(3) . . ? C9 C4 N3 116.9(4) . . ? C9 C4 C5 119.0(4) . . ? N3 C4 C5 123.9(4) . . ? C4 C5 C6 119.7(5) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 118.4(5) . . ? C7 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? C8 C7 C6 122.7(5) . . ? C8 C7 N4 118.6(6) . . ? C6 C7 N4 118.7(6) . . ? C7 C8 C9 118.6(5) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.7 . . ? C8 C9 C4 121.5(4) . . ? C8 C9 H9 119.2 . . ? C4 C9 H9 119.3 . . ? C10 N5 C10 113.0(3) 2_655 . ? C10 N5 C10 113.0(3) 2_655 3_665 ? C10 N5 C10 113.0(3) . 3_665 ? C12 N6 C11 125.2(4) . . ? C12 N6 H6N 117.5 . . ? C11 N6 H6N 117.2 . . ? C12 N7 C13 129.2(4) . . ? C12 N7 H7N 115.0 . . ? C13 N7 H7N 115.8 . . ? O4 N8 O3 118.2(11) . . ? O4 N8 C16 118.9(9) . . ? O3 N8 C16 122.8(11) . . ? N5 C10 C11 110.8(5) . . ? N5 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N5 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? N6 C11 C10 111.4(5) . . ? N6 C11 H11A 109.3 . . ? C10 C11 H11A 109.4 . . ? N6 C11 H11B 109.4 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? N6 C12 N7 113.5(4) . . ? N6 C12 S2 122.9(4) . . ? N7 C12 S2 123.5(4) . . ? O5 P1 O6 109.45(11) . 3_565 ? O5 P1 O6 109.45(12) . 2_665 ? O6 P1 O6 109.49(11) 3_565 2_665 ? O5 P1 O6 109.45(11) . . ? O6 P1 O6 109.49(12) 3_565 . ? O6 P1 O6 109.49(11) 2_665 . ? C19 N9 C23 105.9(11) . . ? C19 N9 C21 118.2(11) . . ? C23 N9 C21 103.3(10) . . ? C19 N9 C25 113.2(11) . . ? C23 N9 C25 103.7(10) . . ? C21 N9 C25 110.8(10) . . ? C21 C22 H22A 109.3 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.6 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N9 C19 C20 117.8(16) . . ? N9 C19 H19A 107.8 . . ? C20 C19 H19A 107.9 . . ? N9 C19 H19B 107.8 . . ? C20 C19 H19B 107.9 . . ? H19A C19 H19B 107.2 . . ? C23 C24 H24A 109.6 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C20 H20A 109.0 . . ? C19 C20 H20B 109.0 . . ? H20A C20 H20B 110.0 . . ? C19 C20 H20C 109.0 . . ? H20A C20 H20C 108.1 . . ? H20B C20 H20C 108.1 . . ? N9 C21 C22 118.4(12) . . ? N9 C21 H21A 108.0 . . ? C22 C21 H21A 107.8 . . ? N9 C21 H21B 107.5 . . ? C22 C21 H21B 107.6 . . ? H21A C21 H21B 107.1 . . ? C26 C25 N9 87(2) . . ? C26 C25 H25A 115.0 . . ? N9 C25 H25A 114.3 . . ? C26 C25 H25B 113.2 . . ? N9 C25 H25B 114.1 . . ? H25A C25 H25B 111.3 . . ? N9 C23 C24 117.9(12) . . ? N9 C23 H23A 107.8 . . ? C24 C23 H23A 107.8 . . ? N9 C23 H23B 107.8 . . ? C24 C23 H23B 107.9 . . ? H23A C23 H23B 107.2 . . ? C25 C26 H26A 109.0 . . ? C25 C26 H26B 109.0 . . ? H26A C26 H26B 109.0 . . ? C25 C26 H26C 108.9 . . ? H26A C26 H26C 110.0 . . ? H26B C26 H26C 109.1 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.78 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.858 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.191 data_Carbonate _database_code_depnum_ccdc_archive 'CCDC 873077' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C27 H30 N10 O6 S3), 2(C8 H20 N), C O3' _chemical_formula_sum 'C71 H100 N22 O15 S6' _chemical_formula_weight 1694.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.2809(7) _cell_length_b 19.0630(7) _cell_length_c 24.6347(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.323(3) _cell_angle_gamma 90.00 _cell_volume 8595.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9984 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 20.13 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 0.232 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.907 _exptl_absorpt_correction_T_max 0.937 _exptl_absorpt_process_details SADABS _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 omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61244 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 24.78 _reflns_number_total 7338 _reflns_number_gt 3976 _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 'Mercury 2.3' _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. Appropriate bond restraints have been applied in SHELXL-97 to ensure standard bond geometry of the receptor molecule and tetraethylammonium cation. ; _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^)+(0.3000P)^2^+0.3500P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7338 _refine_ls_number_parameters 495 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1461 _refine_ls_R_factor_gt 0.0962 _refine_ls_wR_factor_ref 0.2487 _refine_ls_wR_factor_gt 0.2088 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.014 _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 C13 C -0.21972(16) 0.25504(19) 0.28275(14) 0.0796(13) Uani 1 1 d G . . C14 C -0.2740(2) 0.29335(19) 0.29538(17) 0.0993(16) Uani 1 1 d G . . H14 H -0.2618 0.3248 0.3258 0.119 Uiso 1 1 calc R . . C15 C -0.3467(2) 0.2847(2) 0.2625(2) 0.123(2) Uani 1 1 d G . . H15 H -0.3831 0.3104 0.2710 0.148 Uiso 1 1 calc R . . C16 C -0.36505(16) 0.2378(3) 0.2171(2) 0.123(2) Uani 1 1 d G . . C17 C -0.3107(2) 0.1994(2) 0.20443(18) 0.127(2) Uani 1 1 d G . . H17 H -0.3230 0.1680 0.1740 0.152 Uiso 1 1 calc R . . C18 C -0.23807(19) 0.2081(2) 0.23728(17) 0.1057(18) Uani 1 1 d G . . H18 H -0.2017 0.1824 0.2288 0.127 Uiso 1 1 calc R . . C22 C 0.0806(2) 0.0300(2) 0.20996(12) 0.0814(14) Uani 1 1 d G . . C23 C 0.0847(2) 0.06647(19) 0.16223(16) 0.110(2) Uani 1 1 d G . . H23 H 0.0952 0.1142 0.1648 0.132 Uiso 1 1 calc R . . C24 C 0.0733(3) 0.0316(3) 0.11060(12) 0.131(3) Uani 1 1 d G . . H24 H 0.0761 0.0560 0.0787 0.158 Uiso 1 1 calc R . . C25 C 0.0577(3) -0.0398(3) 0.10671(16) 0.137(3) Uani 1 1 d G . . C26 C 0.0535(3) -0.0762(2) 0.1544(2) 0.164(4) Uani 1 1 d G . . H26 H 0.0430 -0.1240 0.1518 0.197 Uiso 1 1 calc R . . C27 C 0.0649(3) -0.0413(2) 0.20607(18) 0.1110(19) Uani 1 1 d G . . H27 H 0.0621 -0.0658 0.2380 0.133 Uiso 1 1 calc R . . N1 N 0.1144(2) 0.2287(2) 0.41476(17) 0.0858(12) Uani 1 1 d . . . C4 C 0.1218(3) 0.4366(2) 0.2182(2) 0.0851(14) Uani 1 1 d . . . C3 C 0.1787(3) 0.3797(3) 0.3136(2) 0.0836(14) Uani 1 1 d . . . C5 C 0.1821(3) 0.4698(3) 0.2093(3) 0.1011(17) Uani 1 1 d . . . H5 H 0.2286 0.4622 0.2347 0.121 Uiso 1 1 calc R . . C7 C 0.1071(5) 0.5226(4) 0.1248(3) 0.117(2) Uani 1 1 d . . . C9 C 0.0545(4) 0.4456(4) 0.1774(3) 0.1095(18) Uani 1 1 d . . . H9 H 0.0141 0.4223 0.1814 0.131 Uiso 1 1 calc R . . C2 C 0.2130(3) 0.3019(4) 0.3972(3) 0.121(2) Uani 1 1 d . . . H2A H 0.2626 0.2988 0.3958 0.145 Uiso 1 1 calc R . . H2B H 0.2121 0.3371 0.4254 0.145 Uiso 1 1 calc R . . C1 C 0.1922(4) 0.2348(6) 0.4149(3) 0.156(3) Uani 1 1 d . . . H1A H 0.2241 0.2250 0.4533 0.187 Uiso 1 1 calc R . . H1B H 0.2008 0.1989 0.3899 0.187 Uiso 1 1 calc R . . C6 C 0.1733(4) 0.5126(3) 0.1640(3) 0.113(2) Uani 1 1 d . . . H6 H 0.2137 0.5357 0.1596 0.135 Uiso 1 1 calc R . . C8 C 0.0461(5) 0.4887(4) 0.1307(4) 0.138(3) Uani 1 1 d . . . H8 H 0.0004 0.4948 0.1036 0.166 Uiso 1 1 calc R . . N3 N 0.1245(2) 0.3923(2) 0.26227(17) 0.0799(11) Uani 1 1 d . . . H3 H 0.0856 0.3677 0.2573 0.096 Uiso 1 1 calc R . . N2 N 0.1652(2) 0.3243(3) 0.34147(18) 0.1002(14) Uani 1 1 d . . . H2 H 0.1262 0.3004 0.3258 0.120 Uiso 1 1 calc R . . N4 N 0.0964(7) 0.5710(4) 0.0777(4) 0.161(3) Uani 1 1 d . . . S1 S 0.25499(10) 0.42647(11) 0.34026(8) 0.1226(7) Uani 1 1 d . . . O2 O 0.1509(5) 0.6050(4) 0.0761(3) 0.177(3) Uani 1 1 d . . . O1 O 0.0350(6) 0.5735(4) 0.0401(3) 0.210(4) Uani 1 1 d . . . C12 C -0.1102(3) 0.2740(3) 0.3691(2) 0.0864(15) Uani 1 1 d . . . C11 C 0.0131(4) 0.2839(5) 0.4408(3) 0.125(3) Uani 1 1 d . . . H11A H 0.0043 0.2470 0.4649 0.150 Uiso 1 1 calc R . . H11B H 0.0036 0.3284 0.4562 0.150 Uiso 1 1 calc R . . C10 C 0.0918(6) 0.2817(6) 0.4434(3) 0.170(4) Uani 1 1 d . . . H10A H 0.1032 0.3260 0.4288 0.204 Uiso 1 1 calc R . . H10B H 0.1211 0.2790 0.4833 0.204 Uiso 1 1 calc R . . N6 N -0.1465(2) 0.2601(2) 0.31263(16) 0.0823(11) Uani 1 1 d . . . H6A H -0.1182 0.2534 0.2922 0.099 Uiso 1 1 calc R . . N5 N -0.0380(3) 0.2757(2) 0.38310(16) 0.0911(13) Uani 1 1 d . . . H5A H -0.0196 0.2716 0.3557 0.109 Uiso 1 1 calc R . . N7 N -0.4396(4) 0.2247(5) 0.1836(4) 0.171(3) Uani 1 1 d D . . S2 S -0.15298(12) 0.28461(17) 0.41786(8) 0.1564(10) Uani 1 1 d . . . O3 O -0.4863(4) 0.2638(5) 0.1934(4) 0.215(4) Uani 1 1 d D . . O4 O -0.4534(4) 0.1782(6) 0.1460(5) 0.261(5) Uani 1 1 d D . . C21 C 0.1086(2) 0.0520(3) 0.3144(2) 0.0749(12) Uani 1 1 d . . . C20 C 0.1216(4) 0.0986(3) 0.4090(2) 0.1073(19) Uani 1 1 d . . . H20A H 0.0954 0.0606 0.4201 0.129 Uiso 1 1 calc R . . H20B H 0.1733 0.0876 0.4232 0.129 Uiso 1 1 calc R . . C19 C 0.1092(6) 0.1608(4) 0.4354(3) 0.153(3) Uani 1 1 d . . . H19A H 0.0603 0.1569 0.4382 0.184 Uiso 1 1 calc R . . H19B H 0.1424 0.1595 0.4742 0.184 Uiso 1 1 calc R . . N9 N 0.0877(2) 0.0699(2) 0.25822(15) 0.0755(10) Uani 1 1 d . . . H9A H 0.0771 0.1135 0.2516 0.091 Uiso 1 1 calc R . . N8 N 0.0993(2) 0.1024(2) 0.34725(15) 0.0839(12) Uani 1 1 d . . . H8A H 0.0784 0.1403 0.3312 0.101 Uiso 1 1 calc R . . S3 S 0.14490(10) -0.02658(9) 0.34100(7) 0.1111(7) Uani 1 1 d . . . N11 N 0.1863(4) 0.6082(3) 0.4291(3) 0.1176(17) Uani 1 1 d . . . C30 C 0.1275(5) 0.6568(5) 0.4332(4) 0.145(3) Uani 1 1 d D . . H30A H 0.1248 0.6543 0.4718 0.174 Uiso 1 1 calc R . . H30B H 0.0813 0.6398 0.4077 0.174 Uiso 1 1 calc R . . C28 C 0.1702(9) 0.5380(8) 0.4384(4) 0.221(6) Uani 1 1 d D . . H28A H 0.2054 0.5088 0.4282 0.265 Uiso 1 1 calc R . . H28B H 0.1227 0.5274 0.4113 0.265 Uiso 1 1 calc R . . C32 C 0.1933(7) 0.6134(6) 0.3681(5) 0.178(4) Uani 1 1 d D . . H32A H 0.2093 0.6602 0.3625 0.214 Uiso 1 1 calc R . . H32B H 0.2303 0.5806 0.3650 0.214 Uiso 1 1 calc R . . C29 C 0.1688(11) 0.5144(10) 0.4965(5) 0.276(8) Uani 1 1 d D . . H29A H 0.2013 0.5432 0.5255 0.414 Uiso 1 1 calc R . . H29B H 0.1841 0.4664 0.5025 0.414 Uiso 1 1 calc R . . H29C H 0.1200 0.5187 0.4985 0.414 Uiso 1 1 calc R . . C31 C 0.1354(5) 0.7329(5) 0.4192(4) 0.166(3) Uani 1 1 d D . . H31A H 0.1789 0.7518 0.4460 0.249 Uiso 1 1 calc R . . H31B H 0.0937 0.7587 0.4214 0.249 Uiso 1 1 calc R . . H31C H 0.1387 0.7365 0.3812 0.249 Uiso 1 1 calc R . . C33 C 0.1225(8) 0.5977(7) 0.3217(5) 0.269(9) Uani 1 1 d D . . H33A H 0.1073 0.5507 0.3262 0.404 Uiso 1 1 calc R . . H33B H 0.1295 0.6024 0.2850 0.404 Uiso 1 1 calc R . . H33C H 0.0856 0.6301 0.3244 0.404 Uiso 1 1 calc R . . C34 C 1.0000 0.2447(4) 0.2500 0.0653(15) Uani 1 2 d S . . O8 O 0.9442(2) 0.2136(2) 0.2515(2) 0.1079(13) Uani 1 1 d . . . O7 O 1.0000 0.3105(3) 0.2500 0.165(4) Uani 1 2 d S . . C35 C 0.2557(6) 0.6308(7) 0.4728(6) 0.189(4) Uani 1 1 d D . . H35A H 0.2471 0.6303 0.5096 0.227 Uiso 1 1 calc R . . H35B H 0.2638 0.6794 0.4647 0.227 Uiso 1 1 calc R . . C36 C 0.3264(8) 0.5921(9) 0.4804(11) 0.321(12) Uani 1 1 d D . . H36A H 0.3271 0.5498 0.5016 0.482 Uiso 1 1 calc R . . H36B H 0.3668 0.6214 0.5007 0.482 Uiso 1 1 calc R . . H36C H 0.3304 0.5806 0.4435 0.482 Uiso 1 1 calc R . . N10 N 0.0470(5) -0.0766(5) 0.0530(4) 0.203(5) Uani 1 1 d DU . . O6 O 0.0685(6) -0.0461(5) 0.0164(3) 0.246(5) Uani 1 1 d DU . . O5 O 0.0246(6) -0.1384(6) 0.0508(4) 0.322(9) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C13 0.085(3) 0.079(3) 0.083(3) 0.001(2) 0.039(3) -0.007(3) C14 0.110(5) 0.100(4) 0.099(4) 0.003(3) 0.049(3) 0.011(3) C15 0.106(5) 0.140(6) 0.139(6) 0.034(5) 0.059(4) 0.036(4) C16 0.080(4) 0.131(6) 0.162(7) 0.025(5) 0.043(4) 0.012(4) C17 0.106(5) 0.126(5) 0.134(5) -0.022(4) 0.019(4) -0.011(4) C18 0.082(4) 0.116(5) 0.115(4) -0.027(4) 0.026(3) 0.007(3) C22 0.068(3) 0.096(4) 0.079(3) -0.015(3) 0.021(2) 0.015(2) C23 0.133(5) 0.122(5) 0.067(3) 0.004(3) 0.021(3) 0.046(4) C24 0.162(7) 0.156(7) 0.069(3) -0.010(4) 0.026(4) 0.068(5) C25 0.104(5) 0.197(9) 0.096(4) -0.053(5) 0.010(4) 0.049(5) C26 0.123(6) 0.160(8) 0.205(10) -0.098(8) 0.044(6) -0.006(5) C27 0.116(5) 0.117(5) 0.105(4) -0.024(4) 0.042(3) 0.010(4) N1 0.083(3) 0.100(3) 0.069(2) 0.003(2) 0.0152(19) -0.019(2) C4 0.101(4) 0.063(3) 0.101(4) -0.003(3) 0.046(3) 0.010(3) C3 0.085(3) 0.089(3) 0.086(3) -0.009(3) 0.039(3) -0.012(3) C5 0.093(4) 0.097(4) 0.123(4) 0.028(3) 0.048(3) 0.006(3) C7 0.150(7) 0.104(5) 0.112(5) 0.020(4) 0.063(5) 0.020(5) C9 0.101(5) 0.109(4) 0.112(4) 0.017(4) 0.024(4) 0.002(3) C2 0.091(4) 0.163(6) 0.101(4) 0.032(4) 0.021(3) -0.038(4) C1 0.096(5) 0.266(11) 0.084(4) 0.013(5) -0.003(3) -0.008(6) C6 0.124(5) 0.104(4) 0.129(5) 0.027(4) 0.066(5) 0.013(4) C8 0.113(6) 0.134(6) 0.153(7) 0.039(5) 0.020(5) 0.013(5) N3 0.074(2) 0.081(3) 0.088(3) -0.001(2) 0.029(2) -0.010(2) N2 0.081(3) 0.122(4) 0.085(3) 0.014(3) 0.007(2) -0.030(3) N4 0.241(10) 0.128(6) 0.140(6) 0.042(5) 0.096(7) 0.013(6) S1 0.1015(12) 0.1406(16) 0.1218(13) -0.0089(10) 0.0294(10) -0.0487(10) O2 0.231(8) 0.155(5) 0.165(5) 0.059(4) 0.092(5) 0.015(5) O1 0.277(10) 0.191(7) 0.130(5) 0.057(5) 0.019(6) 0.024(6) C12 0.108(4) 0.094(4) 0.069(3) -0.014(2) 0.045(3) -0.012(3) C11 0.123(5) 0.183(7) 0.081(4) -0.061(4) 0.051(4) -0.059(5) C10 0.193(9) 0.199(9) 0.081(4) -0.058(5) -0.009(5) 0.032(7) N6 0.091(3) 0.095(3) 0.074(2) -0.013(2) 0.044(2) -0.013(2) N5 0.104(3) 0.112(3) 0.067(2) -0.026(2) 0.041(2) -0.020(2) N7 0.084(5) 0.210(9) 0.205(9) 0.025(7) 0.024(5) 0.010(5) S2 0.1372(16) 0.264(3) 0.0913(11) -0.0381(13) 0.0696(11) -0.0236(16) O3 0.106(4) 0.295(10) 0.236(8) 0.022(7) 0.043(5) 0.033(5) O4 0.113(5) 0.259(10) 0.330(12) -0.066(9) -0.046(6) 0.013(6) C21 0.065(3) 0.092(3) 0.072(3) 0.001(3) 0.027(2) 0.002(2) C20 0.148(5) 0.115(5) 0.055(3) 0.004(3) 0.026(3) -0.016(4) C19 0.280(11) 0.120(6) 0.061(3) 0.013(4) 0.055(5) 0.020(6) N9 0.082(3) 0.079(2) 0.064(2) -0.0012(18) 0.0221(18) 0.0119(19) N8 0.105(3) 0.086(3) 0.057(2) 0.0107(19) 0.0200(19) 0.006(2) S3 0.1153(13) 0.1010(12) 0.1112(12) 0.0188(8) 0.0271(9) 0.0262(9) N11 0.133(5) 0.121(4) 0.118(4) -0.007(3) 0.068(4) -0.013(3) C30 0.134(6) 0.193(10) 0.117(5) -0.011(5) 0.053(4) 0.013(6) C28 0.231(14) 0.216(13) 0.196(12) 0.032(9) 0.038(9) -0.058(10) C32 0.240(12) 0.172(9) 0.164(8) -0.005(7) 0.123(9) 0.025(8) C29 0.34(2) 0.33(2) 0.165(11) 0.075(12) 0.084(12) -0.028(16) C31 0.157(8) 0.163(9) 0.157(8) -0.027(6) 0.019(6) 0.005(6) C33 0.50(3) 0.191(11) 0.109(7) -0.011(7) 0.080(12) 0.076(14) C34 0.074(4) 0.077(4) 0.049(3) 0.000 0.025(3) 0.000 O8 0.110(3) 0.092(2) 0.155(3) -0.031(2) 0.090(3) -0.028(2) O7 0.074(4) 0.075(4) 0.357(12) 0.000 0.086(5) 0.000 C35 0.131(7) 0.211(11) 0.210(10) 0.002(8) 0.030(7) -0.005(7) C36 0.220(17) 0.230(17) 0.51(4) 0.06(2) 0.11(2) 0.037(14) N10 0.191(9) 0.247(11) 0.141(7) -0.097(7) 0.011(6) 0.090(8) O6 0.311(11) 0.305(11) 0.102(4) -0.058(6) 0.038(5) 0.137(9) O5 0.264(11) 0.394(17) 0.317(14) -0.280(15) 0.104(9) -0.057(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C13 N6 1.376(5) . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C16 N7 1.437(9) . ? C17 C18 1.3900 . ? C22 N9 1.381(4) . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C25 N10 1.453(9) . ? C26 C27 1.3900 . ? N1 C10 1.379(9) . ? N1 C19 1.406(8) . ? N1 C1 1.503(9) . ? C4 N3 1.364(6) . ? C4 C9 1.380(8) . ? C4 C5 1.400(8) . ? C3 N2 1.329(6) . ? C3 N3 1.384(6) . ? C3 S1 1.668(5) . ? C5 C6 1.349(8) . ? C7 C6 1.349(10) . ? C7 C8 1.389(11) . ? C7 N4 1.446(10) . ? C9 C8 1.381(10) . ? C2 C1 1.449(12) . ? C2 N2 1.455(7) . ? N4 O2 1.247(11) . ? N4 O1 1.254(13) . ? C12 N5 1.326(7) . ? C12 N6 1.373(6) . ? C12 S2 1.668(5) . ? C11 N5 1.461(8) . ? C11 C10 1.499(13) . ? N7 O4 1.2494(10) . ? N7 O3 1.2494(10) . ? C21 N8 1.306(6) . ? C21 N9 1.357(6) . ? C21 S3 1.695(5) . ? C20 C19 1.407(9) . ? C20 N8 1.448(6) . ? N11 C28 1.408(14) . ? N11 C30 1.492(10) . ? N11 C35 1.493(12) . ? N11 C32 1.553(11) . ? C30 C31 1.5100(10) . ? C28 C29 1.5094(10) . ? C32 C33 1.5099(10) . ? C34 O8 1.238(4) 2_755 ? C34 O8 1.238(4) . ? C34 O7 1.254(8) . ? C35 C36 1.5099(10) . ? N10 O5 1.2496(10) . ? N10 O6 1.2496(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 N6 C13 C14 124.2(3) . . ? N6 C13 C18 115.8(3) . . ? C14 C13 C18 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 N7 118.0(5) . . ? C15 C16 N7 122.0(5) . . ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? N9 C22 C23 115.9(3) . . ? N9 C22 C27 124.0(3) . . ? C23 C22 C27 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 N10 119.9(6) . . ? C24 C25 N10 120.1(6) . . ? C25 C26 C27 120.0 . . ? C26 C27 C22 120.0 . . ? C10 N1 C19 114.8(7) . . ? C10 N1 C1 114.7(7) . . ? C19 N1 C1 104.8(7) . . ? N3 C4 C9 116.7(5) . . ? N3 C4 C5 125.3(5) . . ? C9 C4 C5 117.8(5) . . ? N2 C3 N3 113.3(4) . . ? N2 C3 S1 120.8(4) . . ? N3 C3 S1 125.9(4) . . ? C6 C5 C4 120.5(6) . . ? C6 C7 C8 120.1(6) . . ? C6 C7 N4 121.9(9) . . ? C8 C7 N4 117.9(9) . . ? C4 C9 C8 121.3(7) . . ? C1 C2 N2 112.9(5) . . ? C2 C1 N1 116.0(8) . . ? C7 C6 C5 121.5(7) . . ? C9 C8 C7 118.7(7) . . ? C4 N3 C3 131.6(4) . . ? C3 N2 C2 123.4(5) . . ? O2 N4 O1 124.4(8) . . ? O2 N4 C7 116.7(11) . . ? O1 N4 C7 118.8(10) . . ? N5 C12 N6 115.2(4) . . ? N5 C12 S2 121.8(4) . . ? N6 C12 S2 122.9(4) . . ? N5 C11 C10 113.8(5) . . ? N1 C10 C11 118.5(8) . . ? C12 N6 C13 131.7(4) . . ? C12 N5 C11 126.0(4) . . ? O4 N7 O3 124.7(10) . . ? O4 N7 C16 119.3(7) . . ? O3 N7 C16 115.9(8) . . ? N8 C21 N9 113.1(4) . . ? N8 C21 S3 122.1(4) . . ? N9 C21 S3 124.8(4) . . ? C19 C20 N8 113.9(5) . . ? N1 C19 C20 124.6(6) . . ? C21 N9 C22 131.0(4) . . ? C21 N8 C20 124.2(5) . . ? C28 N11 C30 111.6(8) . . ? C28 N11 C35 110.6(9) . . ? C30 N11 C35 107.4(7) . . ? C28 N11 C32 107.9(7) . . ? C30 N11 C32 108.9(7) . . ? C35 N11 C32 110.4(8) . . ? N11 C30 C31 116.6(7) . . ? N11 C28 C29 120.5(12) . . ? C33 C32 N11 112.8(8) . . ? O8 C34 O8 122.9(7) 2_755 . ? O8 C34 O7 118.5(3) 2_755 . ? O8 C34 O7 118.5(3) . . ? N11 C35 C36 121.2(13) . . ? O5 N10 O6 126.5(9) . . ? O5 N10 C25 116.3(8) . . ? O6 N10 C25 116.6(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.78 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.880 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.065 data_sulfate _database_code_depnum_ccdc_archive 'CCDC 873078' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H30 N10 O6 S3, 2(C16 H36 N), O4 S' _chemical_formula_sum 'C59 H102 N12 O10 S4' _chemical_formula_weight 1267.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.0884(19) _cell_length_b 14.6094(13) _cell_length_c 24.4952(19) _cell_angle_alpha 90.00 _cell_angle_beta 101.722(5) _cell_angle_gamma 90.00 _cell_volume 7038.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4995 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 18.17 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 0.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.924 _exptl_absorpt_correction_T_max 0.954 _exptl_absorpt_process_details SADABS _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 omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35275 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 19.22 _reflns_number_total 5664 _reflns_number_gt 4857 _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 'Mercury 2.3' _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. Appropriate bond restraints have been applied in SHELXL-97 to ensure standard bond geometry of the tetrabutylammonium cations. ; _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^)+(0.1200P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5664 _refine_ls_number_parameters 774 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1741 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S4 S 0.35311(11) 0.32957(15) 0.04576(9) 0.0636(7) Uani 1 1 d . . . S1 S 0.31749(10) -0.07345(13) 0.09079(8) 0.0864(7) Uani 1 1 d . . . S2 S 0.43745(10) 0.33704(14) 0.29929(9) 0.0929(8) Uani 1 1 d . . . S3 S 0.04802(11) 0.29618(16) 0.02298(9) 0.1093(9) Uani 1 1 d . . . N1 N 0.2489(4) 0.1867(5) 0.1878(3) 0.0717(17) Uani 1 1 d . . . C4 C 0.3088(5) 0.0273(8) -0.0269(5) 0.055(2) Uani 1 1 d . . . C9 C 0.3342(3) 0.0670(5) -0.0692(6) 0.069(2) Uani 1 1 d . . . H9 H 0.3616 0.1185 -0.0612 0.082 Uiso 1 1 calc R . . C8 C 0.3207(5) 0.0337(9) -0.1231(5) 0.083(3) Uani 1 1 d . . . H8 H 0.3395 0.0616 -0.1505 0.100 Uiso 1 1 calc R . . C2 C 0.3409(4) 0.0833(5) 0.1745(4) 0.079(2) Uani 1 1 d . . . H2A H 0.3720 0.1265 0.1965 0.094 Uiso 1 1 calc R . . H2B H 0.3588 0.0222 0.1832 0.094 Uiso 1 1 calc R . . C1 C 0.2725(5) 0.0911(6) 0.1898(3) 0.087(2) Uani 1 1 d . . . H1A H 0.2399 0.0545 0.1642 0.105 Uiso 1 1 calc R . . H1B H 0.2751 0.0670 0.2270 0.105 Uiso 1 1 calc R . . C7 C 0.2790(6) -0.0411(9) -0.1356(5) 0.072(3) Uani 1 1 d . . . C3 C 0.3261(3) 0.0386(5) 0.0768(5) 0.062(2) Uani 1 1 d . . . C6 C 0.2529(4) -0.0811(5) -0.0949(6) 0.095(3) Uani 1 1 d . . . H6 H 0.2248 -0.1318 -0.1032 0.114 Uiso 1 1 calc R . . C5 C 0.2676(5) -0.0474(8) -0.0405(5) 0.084(3) Uani 1 1 d . . . H5 H 0.2490 -0.0760 -0.0131 0.100 Uiso 1 1 calc R . . N2 N 0.3366(3) 0.1015(4) 0.1163(4) 0.0680(17) Uani 1 1 d . . . H2 H 0.3413 0.1572 0.1064 0.082 Uiso 1 1 calc R . . N3 N 0.3244(3) 0.0713(4) 0.0245(4) 0.0654(17) Uani 1 1 d . . . H3 H 0.3346 0.1283 0.0229 0.078 Uiso 1 1 calc R . . N4 N 0.2609(5) -0.0784(7) -0.1908(4) 0.112(3) Uani 1 1 d . . . O2 O 0.2202(5) -0.1374(6) -0.2005(3) 0.216(5) Uani 1 1 d . . . O1 O 0.2838(4) -0.0487(6) -0.2256(3) 0.191(4) Uani 1 1 d . . . C16 C 0.6723(7) 0.3367(5) 0.2126(6) 0.083(3) Uani 1 1 d . . . C13 C 0.5306(7) 0.3398(5) 0.2037(6) 0.065(2) Uani 1 1 d . . . C12 C 0.4160(7) 0.3397(4) 0.2297(3) 0.066(2) Uani 1 1 d . . . C14 C 0.5611(7) 0.3222(5) 0.1574(4) 0.078(3) Uani 1 1 d . . . H14 H 0.5332 0.3114 0.1228 0.094 Uiso 1 1 calc R . . C11 C 0.2929(4) 0.3328(6) 0.2293(3) 0.082(2) Uani 1 1 d . . . H11A H 0.2537 0.3615 0.2060 0.098 Uiso 1 1 calc R . . H11B H 0.3029 0.3655 0.2645 0.098 Uiso 1 1 calc R . . C10 C 0.2761(4) 0.2346(6) 0.2399(3) 0.076(2) Uani 1 1 d . . . H10A H 0.3169 0.2036 0.2592 0.091 Uiso 1 1 calc R . . H10B H 0.2430 0.2329 0.2637 0.091 Uiso 1 1 calc R . . C18 C 0.5742(8) 0.3553(4) 0.2541(5) 0.072(2) Uani 1 1 d . . . H18 H 0.5566 0.3673 0.2857 0.086 Uiso 1 1 calc R . . C17 C 0.6436(8) 0.3531(5) 0.2581(5) 0.079(2) Uani 1 1 d . . . H17 H 0.6719 0.3630 0.2927 0.094 Uiso 1 1 calc R . . C15 C 0.6302(8) 0.3206(5) 0.1619(6) 0.092(3) Uani 1 1 d . . . H15 H 0.6485 0.3086 0.1307 0.111 Uiso 1 1 calc R . . N6 N 0.4601(6) 0.3420(3) 0.1937(3) 0.0662(17) Uani 1 1 d . . . H6A H 0.4408 0.3455 0.1590 0.079 Uiso 1 1 calc R . . N5 N 0.3510(5) 0.3400(3) 0.2022(3) 0.0726(18) Uani 1 1 d . . . H5A H 0.3431 0.3447 0.1665 0.087 Uiso 1 1 calc R . . C27 C 0.0789(8) 0.4723(9) -0.0416(5) 0.096(3) Uani 1 1 d . . . H27 H 0.0582 0.4765 -0.0110 0.115 Uiso 1 1 calc R . . C21 C 0.1322(4) 0.3123(8) 0.0380(5) 0.073(2) Uani 1 1 d . . . C22 C 0.1367(7) 0.4225(7) -0.0380(6) 0.078(3) Uani 1 1 d . . . C19 C 0.1761(5) 0.1979(5) 0.1697(4) 0.104(3) Uani 1 1 d . . . H19A H 0.1633 0.2578 0.1812 0.125 Uiso 1 1 calc R . . H19B H 0.1533 0.1524 0.1883 0.125 Uiso 1 1 calc R . . C23 C 0.1702(5) 0.4232(7) -0.0814(8) 0.101(3) Uani 1 1 d . . . H23 H 0.2123 0.3946 -0.0771 0.122 Uiso 1 1 calc R . . C20 C 0.1516(4) 0.1885(7) 0.1075(5) 0.124(3) Uani 1 1 d . . . H20A H 0.1693 0.1323 0.0949 0.149 Uiso 1 1 calc R . . H20B H 0.1024 0.1850 0.0989 0.149 Uiso 1 1 calc R . . N9 N 0.1655(3) 0.3731(6) 0.0102(4) 0.0804(19) Uani 1 1 d . . . H9A H 0.2081 0.3817 0.0235 0.097 Uiso 1 1 calc R . . N8 N 0.1736(4) 0.2657(6) 0.0780(3) 0.088(2) Uani 1 1 d . . . H8A H 0.2155 0.2822 0.0868 0.106 Uiso 1 1 calc R . . N11 N 0.4334(3) 0.6687(4) 0.0607(3) 0.0583(16) Uani 1 1 d . . . C33 C 0.4579(3) 0.7820(5) -0.0132(3) 0.064(2) Uani 1 1 d . . . H33A H 0.4159 0.7669 -0.0388 0.076 Uiso 1 1 calc R . . H33B H 0.4933 0.7422 -0.0213 0.076 Uiso 1 1 calc R . . C32 C 0.4495(3) 0.7658(5) 0.0457(3) 0.0576(19) Uani 1 1 d . . . H32A H 0.4135 0.8054 0.0528 0.069 Uiso 1 1 calc R . . H32B H 0.4911 0.7845 0.0708 0.069 Uiso 1 1 calc R . . C28 C 0.3707(5) 0.6331(4) 0.0211(3) 0.071(2) Uani 1 1 d . . . H28A H 0.3625 0.5709 0.0319 0.085 Uiso 1 1 calc R . . H28B H 0.3806 0.6305 -0.0160 0.085 Uiso 1 1 calc R . . C35 C 0.4849(3) 0.9005(5) -0.0811(3) 0.092(2) Uani 1 1 d . . . H35A H 0.5196 0.8616 -0.0902 0.139 Uiso 1 1 calc R . . H35B H 0.4976 0.9634 -0.0838 0.139 Uiso 1 1 calc R . . H35C H 0.4427 0.8891 -0.1067 0.139 Uiso 1 1 calc R . . C29 C 0.3058(4) 0.6878(5) 0.0182(3) 0.080(2) Uani 1 1 d . . . H29A H 0.2939 0.6882 0.0546 0.096 Uiso 1 1 calc R . . H29B H 0.3135 0.7506 0.0082 0.096 Uiso 1 1 calc R . . C31 C 0.1821(4) 0.6984(6) -0.0265(3) 0.114(3) Uani 1 1 d . . . H31A H 0.1653 0.6865 0.0068 0.171 Uiso 1 1 calc R . . H31B H 0.1494 0.6776 -0.0583 0.171 Uiso 1 1 calc R . . H31C H 0.1893 0.7629 -0.0297 0.171 Uiso 1 1 calc R . . C34 C 0.4764(3) 0.8804(5) -0.0219(3) 0.073(2) Uani 1 1 d . . . H34A H 0.5185 0.8950 0.0038 0.088 Uiso 1 1 calc R . . H34B H 0.4412 0.9199 -0.0131 0.088 Uiso 1 1 calc R . . C30 C 0.2479(5) 0.6485(5) -0.0238(3) 0.095(3) Uani 1 1 d . . . H30A H 0.2595 0.6501 -0.0603 0.114 Uiso 1 1 calc R . . H30B H 0.2418 0.5849 -0.0145 0.114 Uiso 1 1 calc R . . C37 C 0.4103(4) 0.5793(5) 0.1454(3) 0.082(2) Uani 1 1 d . . . H37A H 0.3685 0.5527 0.1247 0.098 Uiso 1 1 calc R . . H37B H 0.4473 0.5381 0.1426 0.098 Uiso 1 1 calc R . . C40 C 0.4915(4) 0.6051(4) 0.0550(3) 0.071(2) Uani 1 1 d . . . H40A H 0.4776 0.5427 0.0602 0.085 Uiso 1 1 calc R . . H40B H 0.4990 0.6100 0.0172 0.085 Uiso 1 1 calc R . . C41 C 0.5580(4) 0.6227(5) 0.0947(3) 0.081(2) Uani 1 1 d . . . H41A H 0.5503 0.6255 0.1325 0.097 Uiso 1 1 calc R . . H41B H 0.5761 0.6812 0.0861 0.097 Uiso 1 1 calc R . . C36 C 0.4223(3) 0.6712(5) 0.1199(3) 0.063(2) Uani 1 1 d . . . H36A H 0.3836 0.7102 0.1209 0.075 Uiso 1 1 calc R . . H36B H 0.4618 0.6995 0.1432 0.075 Uiso 1 1 calc R . . C38 C 0.4056(5) 0.5899(5) 0.2062(4) 0.092(2) Uani 1 1 d . . . H38A H 0.3781 0.6431 0.2100 0.111 Uiso 1 1 calc R . . H38B H 0.3831 0.5366 0.2176 0.111 Uiso 1 1 calc R . . C42 C 0.6092(5) 0.5476(5) 0.0908(3) 0.092(2) Uani 1 1 d . . . H42A H 0.5886 0.4886 0.0949 0.111 Uiso 1 1 calc R . . H42B H 0.6203 0.5495 0.0541 0.111 Uiso 1 1 calc R . . C39 C 0.4747(5) 0.6005(5) 0.2443(4) 0.124(3) Uani 1 1 d . . . H39A H 0.5020 0.5477 0.2410 0.186 Uiso 1 1 calc R . . H39B H 0.4691 0.6064 0.2822 0.186 Uiso 1 1 calc R . . H39C H 0.4967 0.6542 0.2339 0.186 Uiso 1 1 calc R . . C43 C 0.6729(5) 0.5563(6) 0.1338(4) 0.130(3) Uani 1 1 d . . . H43A H 0.6938 0.6144 0.1298 0.195 Uiso 1 1 calc R . . H43B H 0.7036 0.5079 0.1291 0.195 Uiso 1 1 calc R . . H43C H 0.6624 0.5522 0.1703 0.195 Uiso 1 1 calc R . . N12 N 0.9542(3) 0.2518(5) 0.8389(3) 0.0758(18) Uani 1 1 d . . . C45 C 0.9631(4) 0.3351(7) 0.7488(4) 0.112(3) Uani 1 1 d . . . H45A H 0.9412 0.3910 0.7574 0.135 Uiso 1 1 calc R . . H45B H 1.0116 0.3408 0.7630 0.135 Uiso 1 1 calc R . . C44 C 0.9354(4) 0.2542(6) 0.7754(4) 0.092(2) Uani 1 1 d . . . H44A H 0.9519 0.1985 0.7611 0.110 Uiso 1 1 calc R . . H44B H 0.8863 0.2543 0.7641 0.110 Uiso 1 1 calc R . . C46 C 0.9488(5) 0.3192(7) 0.6870(5) 0.151(4) Uani 1 1 d D . . H46A H 0.9734 0.2650 0.6795 0.181 Uiso 1 1 calc R . . H46B H 0.9007 0.3066 0.6747 0.181 Uiso 1 1 calc R . . C47 C 0.9675(6) 0.3967(7) 0.6529(4) 0.199(5) Uani 1 1 d D . . H47A H 0.9356 0.4458 0.6521 0.298 Uiso 1 1 calc R . . H47B H 0.9666 0.3760 0.6156 0.298 Uiso 1 1 calc R . . H47C H 1.0124 0.4180 0.6692 0.298 Uiso 1 1 calc R . . C48 C 0.9201(4) 0.1669(5) 0.8560(4) 0.085(2) Uani 1 1 d . . . H48A H 0.8717 0.1716 0.8410 0.102 Uiso 1 1 calc R . . H48B H 0.9367 0.1143 0.8386 0.102 Uiso 1 1 calc R . . C49 C 0.9301(4) 0.1484(6) 0.9179(4) 0.095(2) Uani 1 1 d . . . H49A H 0.9784 0.1444 0.9338 0.114 Uiso 1 1 calc R . . H49B H 0.9116 0.1989 0.9358 0.114 Uiso 1 1 calc R . . C50 C 0.8962(4) 0.0614(7) 0.9293(4) 0.118(3) Uani 1 1 d . . . H50A H 0.9150 0.0114 0.9112 0.142 Uiso 1 1 calc R . . H50B H 0.8482 0.0656 0.9126 0.142 Uiso 1 1 calc R . . C51 C 0.9036(4) 0.0392(6) 0.9902(4) 0.144(4) Uani 1 1 d . . . H51A H 0.9509 0.0339 1.0070 0.216 Uiso 1 1 calc R . . H51B H 0.8810 -0.0176 0.9941 0.216 Uiso 1 1 calc R . . H51C H 0.8835 0.0871 1.0082 0.216 Uiso 1 1 calc R . . C52 C 0.9301(4) 0.3374(5) 0.8640(3) 0.081(2) Uani 1 1 d . . . H52A H 0.9522 0.3895 0.8507 0.098 Uiso 1 1 calc R . . H52B H 0.9461 0.3344 0.9040 0.098 Uiso 1 1 calc R . . C53 C 0.8542(4) 0.3570(6) 0.8529(3) 0.098(3) Uani 1 1 d D . . H53A H 0.8353 0.3544 0.8132 0.117 Uiso 1 1 calc R . . H53B H 0.8311 0.3118 0.8714 0.117 Uiso 1 1 calc R . . C54 C 0.8447(4) 0.4509(7) 0.8750(4) 0.166(5) Uani 1 1 d D . . H54A H 0.8699 0.4558 0.9131 0.199 Uiso 1 1 calc R . . H54B H 0.8623 0.4963 0.8527 0.199 Uiso 1 1 calc R . . C55 C 0.7708(5) 0.4685(7) 0.8732(4) 0.201(5) Uani 1 1 d D . . H55A H 0.7465 0.4679 0.8351 0.301 Uiso 1 1 calc R . . H55B H 0.7656 0.5272 0.8894 0.301 Uiso 1 1 calc R . . H55C H 0.7531 0.4218 0.8938 0.301 Uiso 1 1 calc R . . C56 C 1.0306(4) 0.2489(5) 0.8596(3) 0.090(2) Uani 1 1 d . . . H56A H 1.0400 0.2480 0.9000 0.108 Uiso 1 1 calc R . . H56B H 1.0498 0.3049 0.8481 0.108 Uiso 1 1 calc R . . C57 C 1.0672(5) 0.1683(7) 0.8395(5) 0.164(4) Uani 1 1 d D . . H57A H 1.0564 0.1133 0.8581 0.197 Uiso 1 1 calc R . . H57B H 1.0501 0.1603 0.7998 0.197 Uiso 1 1 calc R . . C58 C 1.1430(5) 0.1789(9) 0.8498(6) 0.205(6) Uani 1 1 d D . . H58A H 1.1635 0.1327 0.8300 0.246 Uiso 1 1 calc R . . H58B H 1.1558 0.2391 0.8388 0.246 Uiso 1 1 calc R . . C59 C 1.1632(6) 0.1660(9) 0.9117(6) 0.248(7) Uani 1 1 d D . . H59A H 1.1306 0.1956 0.9295 0.373 Uiso 1 1 calc R . . H59B H 1.2073 0.1924 0.9250 0.373 Uiso 1 1 calc R . . H59C H 1.1647 0.1018 0.9203 0.373 Uiso 1 1 calc R . . O10 O 0.4157(2) 0.3743(3) 0.07236(18) 0.0826(14) Uani 1 1 d . . . O7 O 0.3194(2) 0.2898(3) 0.08994(18) 0.0757(14) Uani 1 1 d . . . O8 O 0.3059(2) 0.3965(3) 0.01437(19) 0.0934(16) Uani 1 1 d . . . O9 O 0.3669(2) 0.2548(3) 0.00968(18) 0.0864(15) Uani 1 1 d . . . C25 C 0.0810(10) 0.5084(9) -0.1356(8) 0.120(4) Uani 1 1 d . . . C26 C 0.0504(6) 0.5174(7) -0.0915(9) 0.109(3) Uani 1 1 d . . . H26 H 0.0114 0.5527 -0.0942 0.130 Uiso 1 1 calc R . . C24 C 0.1425(10) 0.4662(10) -0.1319(6) 0.122(4) Uani 1 1 d . . . H24 H 0.1649 0.4661 -0.1617 0.146 Uiso 1 1 calc R . . N7 N 0.7455(6) 0.3398(5) 0.2158(5) 0.118(3) Uani 1 1 d . . . O3 O 0.7668(4) 0.3319(5) 0.1723(4) 0.155(3) Uani 1 1 d . . . O4 O 0.7805(4) 0.3506(5) 0.2610(4) 0.160(3) Uani 1 1 d . . . N10 N 0.0476(8) 0.5483(9) -0.1911(6) 0.161(5) Uani 1 1 d . . . O6 O -0.0071(6) 0.5902(7) -0.1919(5) 0.224(6) Uani 1 1 d . . . O5 O 0.0773(6) 0.5356(7) -0.2295(4) 0.196(5) 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 S4 0.0741(17) 0.0564(16) 0.0571(16) 0.0058(14) 0.0061(14) -0.0025(14) S1 0.1352(19) 0.0548(17) 0.0698(15) 0.0035(12) 0.0225(13) 0.0079(12) S2 0.1154(18) 0.1086(18) 0.0520(17) -0.0038(12) 0.0104(13) 0.0309(13) S3 0.0802(19) 0.132(2) 0.1063(19) 0.0129(15) -0.0042(14) -0.0245(14) N1 0.093(6) 0.066(6) 0.055(5) -0.002(4) 0.012(4) -0.005(4) C4 0.067(6) 0.065(8) 0.033(8) 0.012(7) 0.016(6) -0.001(6) C9 0.074(6) 0.063(6) 0.062(7) 0.003(8) -0.002(7) -0.014(4) C8 0.090(7) 0.091(8) 0.072(11) 0.014(7) 0.023(6) -0.025(6) C2 0.110(8) 0.060(6) 0.057(7) 0.001(5) -0.004(5) 0.014(5) C1 0.132(8) 0.067(8) 0.058(6) 0.005(5) 0.007(6) -0.018(6) C7 0.098(7) 0.079(8) 0.045(9) 0.025(8) 0.031(7) 0.003(7) C3 0.077(5) 0.056(8) 0.050(8) -0.001(7) 0.005(5) 0.012(4) C6 0.131(8) 0.079(7) 0.065(7) -0.029(8) 0.000(8) -0.043(6) C5 0.097(6) 0.070(7) 0.087(11) 0.010(6) 0.025(6) -0.041(6) N2 0.108(5) 0.049(5) 0.045(5) 0.004(5) 0.009(4) -0.004(3) N3 0.091(5) 0.055(5) 0.047(5) 0.000(5) 0.006(4) -0.006(3) N4 0.181(9) 0.124(8) 0.032(8) -0.013(7) 0.024(6) -0.050(6) O2 0.333(12) 0.214(9) 0.098(6) -0.043(6) 0.039(6) -0.168(8) O1 0.283(9) 0.237(9) 0.067(6) -0.033(5) 0.067(6) -0.098(7) C16 0.102(12) 0.086(6) 0.044(8) -0.007(5) -0.023(12) 0.020(6) C13 0.083(10) 0.051(5) 0.048(9) -0.004(5) -0.016(11) -0.002(5) C12 0.090(8) 0.047(5) 0.060(9) -0.004(4) 0.011(8) 0.017(5) C14 0.117(12) 0.079(6) 0.034(8) -0.014(4) 0.003(8) 0.005(5) C11 0.095(7) 0.072(8) 0.076(6) -0.017(5) 0.012(5) 0.014(5) C10 0.103(6) 0.069(7) 0.060(7) -0.005(6) 0.027(5) 0.007(5) C18 0.081(9) 0.069(6) 0.062(10) -0.012(5) 0.007(8) -0.008(5) C17 0.103(12) 0.074(6) 0.043(9) -0.009(5) -0.021(8) -0.006(5) C15 0.069(9) 0.128(8) 0.081(12) 0.002(6) 0.017(9) 0.022(6) N6 0.080(7) 0.069(4) 0.043(5) -0.004(3) -0.004(6) -0.002(4) N5 0.086(6) 0.061(4) 0.071(5) 0.003(3) 0.017(6) 0.005(4) C27 0.096(10) 0.086(7) 0.091(11) 0.007(7) -0.013(7) -0.005(7) C21 0.063(8) 0.083(7) 0.065(7) -0.014(6) -0.006(7) -0.012(6) C22 0.060(9) 0.072(7) 0.088(12) 0.012(7) -0.020(9) -0.011(7) C19 0.082(8) 0.126(8) 0.104(9) 0.027(6) 0.015(7) -0.015(6) C23 0.093(8) 0.113(9) 0.095(10) 0.014(8) 0.011(11) -0.033(6) C20 0.104(8) 0.136(9) 0.112(9) 0.050(7) -0.024(7) -0.049(6) N9 0.068(5) 0.088(5) 0.077(6) 0.006(5) -0.005(6) -0.020(5) N8 0.074(5) 0.102(6) 0.078(5) 0.020(5) -0.013(5) -0.025(5) N11 0.090(5) 0.034(5) 0.052(5) -0.008(4) 0.017(4) 0.001(4) C33 0.076(5) 0.046(6) 0.070(7) 0.000(4) 0.016(4) -0.003(4) C32 0.071(5) 0.044(6) 0.057(6) -0.008(4) 0.012(4) 0.002(4) C28 0.097(7) 0.048(5) 0.064(6) -0.020(4) 0.008(5) -0.016(6) C35 0.115(6) 0.086(6) 0.077(7) 0.010(5) 0.020(5) 0.000(5) C29 0.092(7) 0.065(6) 0.078(6) -0.008(5) 0.002(6) -0.015(6) C31 0.080(7) 0.110(7) 0.142(8) 0.007(6) -0.003(6) -0.021(6) C34 0.074(5) 0.073(7) 0.068(7) 0.002(5) 0.007(4) 0.000(4) C30 0.090(7) 0.096(7) 0.090(7) -0.013(5) -0.003(6) -0.021(6) C37 0.117(6) 0.053(6) 0.081(7) 0.004(5) 0.033(5) -0.013(4) C40 0.103(7) 0.046(5) 0.065(6) -0.014(4) 0.021(6) 0.017(5) C41 0.096(7) 0.075(6) 0.073(6) -0.015(5) 0.020(6) 0.015(6) C36 0.088(6) 0.060(6) 0.045(6) -0.007(4) 0.022(4) 0.004(4) C38 0.138(8) 0.061(6) 0.092(8) 0.009(5) 0.055(7) -0.011(5) C42 0.112(7) 0.088(7) 0.080(7) -0.001(5) 0.028(6) 0.021(6) C39 0.175(10) 0.103(7) 0.092(7) 0.005(5) 0.023(7) -0.004(6) C43 0.116(8) 0.135(8) 0.136(9) -0.021(6) 0.018(7) 0.032(6) N12 0.072(6) 0.069(6) 0.083(6) -0.015(4) 0.008(4) 0.003(4) C45 0.138(8) 0.117(9) 0.079(8) 0.004(7) 0.015(6) 0.000(6) C44 0.117(7) 0.087(7) 0.068(8) -0.007(6) 0.011(6) -0.002(5) C46 0.185(10) 0.138(10) 0.136(11) 0.033(8) 0.049(8) -0.007(7) C47 0.270(14) 0.178(11) 0.159(11) 0.038(9) 0.070(10) 0.023(10) C48 0.094(6) 0.064(6) 0.094(8) -0.004(5) 0.012(5) -0.023(5) C49 0.102(7) 0.085(7) 0.092(8) -0.001(6) 0.004(6) -0.004(5) C50 0.130(8) 0.099(8) 0.126(10) 0.003(7) 0.028(6) -0.030(6) C51 0.166(9) 0.164(9) 0.119(9) 0.041(7) 0.066(7) 0.005(7) C52 0.084(7) 0.066(6) 0.090(6) -0.014(5) 0.010(5) 0.014(5) C53 0.096(8) 0.117(8) 0.079(6) -0.001(5) 0.014(5) 0.015(6) C54 0.080(7) 0.214(13) 0.196(11) -0.112(9) 0.010(7) 0.052(7) C55 0.294(16) 0.166(11) 0.145(10) 0.008(8) 0.052(10) 0.012(11) C56 0.074(7) 0.085(7) 0.108(7) -0.013(5) 0.009(6) -0.001(5) C57 0.105(9) 0.166(10) 0.206(12) -0.079(8) -0.007(8) 0.055(8) C58 0.183(15) 0.197(13) 0.207(14) -0.013(11) -0.028(12) 0.079(10) C59 0.138(11) 0.223(15) 0.39(2) 0.017(16) 0.061(14) 0.067(9) O10 0.083(4) 0.075(3) 0.080(4) -0.007(3) -0.006(3) -0.022(3) O7 0.100(4) 0.068(3) 0.062(3) 0.009(3) 0.022(3) -0.003(3) O8 0.081(3) 0.101(4) 0.096(4) 0.050(3) 0.012(3) 0.012(3) O9 0.126(4) 0.066(4) 0.077(3) -0.026(3) 0.043(3) -0.019(3) C25 0.118(14) 0.108(10) 0.116(17) 0.033(10) -0.021(13) -0.048(10) C26 0.106(9) 0.071(7) 0.127(12) 0.009(9) -0.026(12) -0.014(6) C24 0.130(13) 0.139(10) 0.083(12) 0.034(8) -0.007(10) -0.070(9) N7 0.061(9) 0.156(7) 0.122(12) -0.020(7) -0.016(10) 0.024(5) O3 0.110(6) 0.229(8) 0.124(7) -0.006(6) 0.021(5) 0.034(5) O4 0.096(6) 0.236(8) 0.127(7) -0.043(6) -0.030(5) 0.029(5) N10 0.208(16) 0.126(10) 0.122(13) 0.072(10) -0.028(13) -0.069(10) O6 0.213(10) 0.198(10) 0.224(11) 0.110(8) -0.045(9) 0.001(7) O5 0.250(11) 0.180(8) 0.122(8) 0.067(7) -0.044(7) -0.085(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S4 O10 1.450(4) . ? S4 O9 1.466(4) . ? S4 O8 1.467(4) . ? S4 O7 1.505(4) . ? S1 C3 1.689(8) . ? S2 C12 1.671(8) . ? S3 C21 1.672(8) . ? N1 C19 1.449(8) . ? N1 C10 1.460(7) . ? N1 C1 1.473(8) . ? C4 C5 1.370(9) . ? C4 C9 1.373(9) . ? C4 N3 1.390(8) . ? C9 C8 1.381(9) . ? C8 C7 1.373(9) . ? C2 N2 1.437(8) . ? C2 C1 1.499(9) . ? C7 C6 1.349(9) . ? C7 N4 1.436(11) . ? C3 N2 1.318(8) . ? C3 N3 1.362(8) . ? C6 C5 1.394(9) . ? N4 O1 1.133(8) . ? N4 O2 1.179(8) . ? C16 C15 1.373(10) . ? C16 C17 1.377(11) . ? C16 N7 1.457(12) . ? C13 C18 1.380(10) . ? C13 N6 1.388(19) . ? C13 C14 1.417(10) . ? C12 N5 1.343(8) . ? C12 N6 1.373(9) . ? C14 C15 1.37(2) . ? C11 N5 1.459(8) . ? C11 C10 1.508(8) . ? C18 C17 1.38(2) . ? C27 C22 1.357(10) . ? C27 C26 1.404(12) . ? C21 N8 1.335(8) . ? C21 N9 1.375(9) . ? C22 C23 1.369(11) . ? C22 N9 1.405(10) . ? C19 C20 1.510(10) . ? C23 C24 1.399(12) . ? C20 N8 1.455(9) . ? N11 C36 1.511(7) . ? N11 C28 1.515(7) . ? N11 C32 1.517(7) . ? N11 C40 1.521(7) . ? C33 C32 1.506(7) . ? C33 C34 1.510(8) . ? C28 C29 1.519(8) . ? C35 C34 1.523(8) . ? C29 C30 1.501(8) . ? C31 C30 1.499(9) . ? C37 C38 1.519(9) . ? C37 C36 1.519(8) . ? C40 C41 1.506(8) . ? C41 C42 1.520(8) . ? C38 C39 1.515(9) . ? C42 C43 1.490(9) . ? N12 C48 1.516(8) . ? N12 C52 1.516(8) . ? N12 C56 1.517(8) . ? N12 C44 1.525(8) . ? C45 C46 1.502(11) . ? C45 C44 1.509(10) . ? C46 C47 1.4992(11) . ? C48 C49 1.514(9) . ? C49 C50 1.494(9) . ? C50 C51 1.504(10) . ? C52 C53 1.520(9) . ? C53 C54 1.5011(11) . ? C54 C55 1.4988(11) . ? C56 C57 1.520(10) . ? C57 C58 1.5007(11) . ? C58 C59 1.4996(11) . ? C25 C26 1.35(3) . ? C25 C24 1.37(3) . ? C25 N10 1.507(18) . ? N7 O4 1.196(9) . ? N7 O3 1.230(10) . ? N10 O5 1.226(14) . ? N10 O6 1.254(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 S4 O9 110.7(3) . . ? O10 S4 O8 110.1(3) . . ? O9 S4 O8 111.2(3) . . ? O10 S4 O7 109.1(3) . . ? O9 S4 O7 108.3(3) . . ? O8 S4 O7 107.3(3) . . ? C19 N1 C10 112.9(7) . . ? C19 N1 C1 114.5(7) . . ? C10 N1 C1 111.4(6) . . ? C5 C4 C9 116.9(8) . . ? C5 C4 N3 127.0(11) . . ? C9 C4 N3 115.9(11) . . ? C4 C9 C8 122.8(8) . . ? C7 C8 C9 119.1(8) . . ? N2 C2 C1 111.1(6) . . ? N1 C1 C2 111.7(6) . . ? C6 C7 C8 119.4(9) . . ? C6 C7 N4 118.1(13) . . ? C8 C7 N4 122.5(12) . . ? N2 C3 N3 114.6(7) . . ? N2 C3 S1 122.3(8) . . ? N3 C3 S1 123.1(7) . . ? C7 C6 C5 121.0(8) . . ? C4 C5 C6 120.9(8) . . ? C3 N2 C2 124.6(7) . . ? C3 N3 C4 130.4(7) . . ? O1 N4 O2 120.0(10) . . ? O1 N4 C7 120.0(11) . . ? O2 N4 C7 120.0(10) . . ? C15 C16 C17 118.6(10) . . ? C15 C16 N7 118.9(13) . . ? C17 C16 N7 122.4(14) . . ? C18 C13 N6 126.5(12) . . ? C18 C13 C14 116.5(9) . . ? N6 C13 C14 117.0(12) . . ? N5 C12 N6 111.5(8) . . ? N5 C12 S2 122.3(9) . . ? N6 C12 S2 126.2(8) . . ? C15 C14 C13 122.3(9) . . ? N5 C11 C10 111.9(6) . . ? N1 C10 C11 111.3(6) . . ? C17 C18 C13 120.7(9) . . ? C18 C17 C16 122.0(9) . . ? C14 C15 C16 119.9(10) . . ? C12 N6 C13 130.9(8) . . ? C12 N5 C11 123.9(8) . . ? C22 C27 C26 120.0(10) . . ? N8 C21 N9 113.5(8) . . ? N8 C21 S3 122.8(9) . . ? N9 C21 S3 123.6(8) . . ? C27 C22 C23 119.7(10) . . ? C27 C22 N9 122.1(14) . . ? C23 C22 N9 118.2(14) . . ? N1 C19 C20 113.5(7) . . ? C22 C23 C24 121.4(11) . . ? N8 C20 C19 111.2(7) . . ? C21 N9 C22 126.2(8) . . ? C21 N8 C20 123.5(8) . . ? C36 N11 C28 111.0(5) . . ? C36 N11 C32 106.8(5) . . ? C28 N11 C32 110.9(5) . . ? C36 N11 C40 111.6(5) . . ? C28 N11 C40 106.6(6) . . ? C32 N11 C40 110.0(5) . . ? C32 C33 C34 111.3(6) . . ? C33 C32 N11 116.7(5) . . ? N11 C28 C29 116.4(6) . . ? C30 C29 C28 111.8(7) . . ? C33 C34 C35 113.3(6) . . ? C31 C30 C29 113.5(7) . . ? C38 C37 C36 111.1(6) . . ? C41 C40 N11 115.6(6) . . ? C40 C41 C42 111.0(6) . . ? N11 C36 C37 116.1(6) . . ? C39 C38 C37 112.5(6) . . ? C43 C42 C41 112.9(7) . . ? C48 N12 C52 111.3(6) . . ? C48 N12 C56 111.6(6) . . ? C52 N12 C56 105.9(6) . . ? C48 N12 C44 105.5(6) . . ? C52 N12 C44 111.2(6) . . ? C56 N12 C44 111.4(6) . . ? C46 C45 C44 107.6(7) . . ? C45 C44 N12 114.9(7) . . ? C47 C46 C45 115.2(9) . . ? C49 C48 N12 116.5(7) . . ? C50 C49 C48 111.4(7) . . ? C49 C50 C51 114.3(8) . . ? N12 C52 C53 118.3(6) . . ? C54 C53 C52 107.6(6) . . ? C55 C54 C53 110.1(8) . . ? N12 C56 C57 115.9(7) . . ? C58 C57 C56 114.0(8) . . ? C59 C58 C57 102.4(10) . . ? C26 C25 C24 122.8(15) . . ? C26 C25 N10 119(2) . . ? C24 C25 N10 118(2) . . ? C25 C26 C27 118.6(12) . . ? C25 C24 C23 116.9(13) . . ? O4 N7 O3 124.7(11) . . ? O4 N7 C16 116.8(12) . . ? O3 N7 C16 118.4(11) . . ? O5 N10 O6 128.7(17) . . ? O5 N10 C25 115.8(17) . . ? O6 N10 C25 115.5(16) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 19.22 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.350 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.044 data_fluoride _database_code_depnum_ccdc_archive 'CCDC 873079' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H30 N10 O6 S3, C16 H36 N, 2(C2 H6 O S), F' _chemical_formula_sum 'C47 H78 F N11 O8 S5' _chemical_formula_weight 1104.55 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.832(3) _cell_length_b 13.5139(14) _cell_length_c 27.699(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.856(7) _cell_angle_gamma 90.00 _cell_volume 11858(2) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9440 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 23.12 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4720 _exptl_absorpt_coefficient_mu 0.255 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.896 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details SADABS _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 omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47212 _diffrn_reflns_av_R_equivalents 0.1125 _diffrn_reflns_av_sigmaI/netI 0.1345 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 28.42 _reflns_number_total 14739 _reflns_number_gt 12704 _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 'Mercury 2.3' _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. Appropriate bond restraints have been applied in SHELXL-97 to ensure standard bond geometry of the lattice DMSO molecules and one of them has been refined isotropically due to disorder. ; _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^)+(0.1700P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14739 _refine_ls_number_parameters 653 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1284 _refine_ls_R_factor_gt 0.0979 _refine_ls_wR_factor_ref 0.2458 _refine_ls_wR_factor_gt 0.1913 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.007 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 0.21183(6) 0.3399(2) 0.21988(7) 0.1287(9) Uani 1 1 d . . . S1 S -0.05770(7) 0.4584(2) 0.08401(9) 0.1307(9) Uani 1 1 d . . . S2 S 0.06736(8) -0.10587(18) 0.15266(9) 0.1272(8) Uani 1 1 d . . . O1 O -0.0591(3) 0.3911(7) -0.1990(3) 0.187(3) Uani 1 1 d . . . O2 O -0.1091(3) 0.4809(7) -0.1996(3) 0.170(3) Uani 1 1 d . . . O3 O 0.0536(2) -0.0505(6) -0.1393(3) 0.150(3) Uani 1 1 d . . . O4 O 0.0574(3) -0.1949(7) -0.1082(3) 0.182(3) Uani 1 1 d . . . O5 O 0.1715(3) 0.2947(8) -0.0805(3) 0.203(4) Uani 1 1 d . . . O6 O 0.2292(3) 0.3575(7) -0.0255(3) 0.178(3) Uani 1 1 d . . . N1 N 0.07159(18) 0.2491(5) 0.2302(2) 0.0894(17) Uani 1 1 d . . . N2 N 0.01522(17) 0.3670(5) 0.1394(2) 0.0957(18) Uani 1 1 d . . . H2N H 0.0376 0.3416 0.1403 0.115 Uiso 1 1 calc R . . N3 N -0.00658(15) 0.3705(4) 0.0498(2) 0.0830(15) Uani 1 1 d D . . H3N H 0.0160 0.3356 0.0607 0.100 Uiso 1 1 calc RD . . N4 N -0.0786(3) 0.4271(7) -0.1762(3) 0.134(3) Uani 1 1 d . . . N5 N 0.05313(18) 0.0830(6) 0.1601(2) 0.0924(17) Uani 1 1 d D . . N6 N 0.05670(16) 0.0458(5) 0.0836(2) 0.0824(15) Uani 1 1 d D . . N7 N 0.0558(2) -0.1074(8) -0.1040(3) 0.116(2) Uani 1 1 d . . . N8 N 0.13530(19) 0.2915(5) 0.2012(2) 0.0875(17) Uani 1 1 d . . . N9 N 0.14181(15) 0.3049(4) 0.12417(19) 0.0795(14) Uani 1 1 d D . . N10 N 0.1948(3) 0.3249(6) -0.0368(3) 0.129(3) Uani 1 1 d . . . C1 C 0.0555(2) 0.3447(7) 0.2384(3) 0.107(2) Uani 1 1 d . . . H1A H 0.0760 0.3959 0.2435 0.129 Uiso 1 1 calc R . . H1B H 0.0527 0.3412 0.2715 0.129 Uiso 1 1 calc R . . C2 C 0.0131(2) 0.3736(6) 0.1909(3) 0.111(2) Uani 1 1 d . . . H2A H -0.0087 0.3297 0.1897 0.133 Uiso 1 1 calc R . . H2B H 0.0060 0.4406 0.1961 0.133 Uiso 1 1 calc R . . C3 C -0.0151(2) 0.3975(5) 0.0913(3) 0.0878(19) Uani 1 1 d . . . C4 C -0.0266(2) 0.3873(5) -0.0064(3) 0.0769(17) Uani 1 1 d . . . C5 C -0.0092(2) 0.3439(5) -0.0355(3) 0.0876(19) Uani 1 1 d . . . H5 H 0.0148 0.3051 -0.0168 0.105 Uiso 1 1 calc R . . C6 C -0.0248(3) 0.3541(6) -0.0904(3) 0.100(2) Uani 1 1 d . . . H6 H -0.0125 0.3218 -0.1090 0.120 Uiso 1 1 calc R . . C7 C -0.0594(3) 0.4136(7) -0.1173(3) 0.102(2) Uani 1 1 d . . . C8 C -0.0779(2) 0.4609(6) -0.0896(3) 0.102(2) Uani 1 1 d . . . H8 H -0.1014 0.5011 -0.1084 0.123 Uiso 1 1 calc R . . C9 C -0.0617(2) 0.4486(5) -0.0347(3) 0.0904(19) Uani 1 1 d . . . H9 H -0.0740 0.4808 -0.0160 0.109 Uiso 1 1 calc R . . C10 C 0.0464(2) 0.1664(7) 0.2337(3) 0.108(2) Uani 1 1 d . . . H10A H 0.0167 0.1819 0.2121 0.129 Uiso 1 1 calc R . . H10B H 0.0521 0.1584 0.2713 0.129 Uiso 1 1 calc R . . C11 C 0.0556(2) 0.0710(7) 0.2138(3) 0.108(2) Uani 1 1 d . . . H11A H 0.0836 0.0483 0.2395 0.129 Uiso 1 1 calc R . . H11B H 0.0355 0.0211 0.2119 0.129 Uiso 1 1 calc R . . C12 C 0.0588(2) 0.0104(6) 0.1312(3) 0.090(2) Uani 1 1 d . . . C13 C 0.05610(17) 0.0014(6) 0.0387(3) 0.0768(17) Uani 1 1 d . . . C14 C 0.05369(18) 0.0632(5) -0.0025(3) 0.0835(18) Uani 1 1 d . . . H14 H 0.0521 0.1310 0.0021 0.100 Uiso 1 1 calc R . . C15 C 0.05354(19) 0.0312(6) -0.0494(3) 0.0885(19) Uani 1 1 d . . . H15 H 0.0523 0.0754 -0.0759 0.106 Uiso 1 1 calc R . . C16 C 0.0553(2) -0.0677(8) -0.0555(3) 0.094(2) Uani 1 1 d . . . C17 C 0.0568(2) -0.1332(6) -0.0167(3) 0.105(2) Uani 1 1 d . . . H17 H 0.0578 -0.2009 -0.0221 0.126 Uiso 1 1 calc R . . C18 C 0.0568(2) -0.0994(7) 0.0299(3) 0.094(2) Uani 1 1 d . . . H18 H 0.0573 -0.1441 0.0557 0.113 Uiso 1 1 calc R . . C19 C 0.1160(2) 0.2385(6) 0.2693(3) 0.103(2) Uani 1 1 d . . . H19A H 0.1241 0.1699 0.2695 0.123 Uiso 1 1 calc R . . H19B H 0.1197 0.2539 0.3054 0.123 Uiso 1 1 calc R . . C20 C 0.1457(2) 0.3034(6) 0.2579(2) 0.098(2) Uani 1 1 d . . . H20A H 0.1424 0.3721 0.2654 0.117 Uiso 1 1 calc R . . H20B H 0.1747 0.2840 0.2812 0.117 Uiso 1 1 calc R . . C21 C 0.16152(18) 0.3127(5) 0.1798(2) 0.0785(17) Uani 1 1 d . . . C22 C 0.15741(18) 0.3159(5) 0.0870(2) 0.0749(17) Uani 1 1 d . . . C23 C 0.1297(2) 0.2949(6) 0.0336(3) 0.097(2) Uani 1 1 d . . . H23 H 0.1021 0.2778 0.0249 0.116 Uiso 1 1 calc R . . C24 C 0.1407(2) 0.2980(6) -0.0078(3) 0.108(2) Uani 1 1 d . . . H24 H 0.1213 0.2826 -0.0435 0.130 Uiso 1 1 calc R . . C25 C 0.1813(3) 0.3245(6) 0.0056(3) 0.098(2) Uani 1 1 d . . . C26 C 0.2092(2) 0.3479(6) 0.0575(3) 0.113(3) Uani 1 1 d . . . H26 H 0.2364 0.3664 0.0655 0.136 Uiso 1 1 calc R . . C27 C 0.1982(2) 0.3451(6) 0.0991(3) 0.108(3) Uani 1 1 d . . . H27 H 0.2177 0.3623 0.1346 0.130 Uiso 1 1 calc R . . N11 N 0.29519(15) 0.4793(5) 0.37752(19) 0.0836(15) Uani 1 1 d . . . C28 C 0.3199(2) 0.5174(6) 0.4360(2) 0.101(2) Uani 1 1 d . . . H28A H 0.3493 0.4992 0.4495 0.121 Uiso 1 1 calc R . . H28B H 0.3185 0.5891 0.4350 0.121 Uiso 1 1 calc R . . C29 C 0.3057(2) 0.4814(7) 0.4764(3) 0.111(2) Uani 1 1 d . . . H29A H 0.2763 0.4983 0.4632 0.133 Uiso 1 1 calc R . . H29B H 0.3083 0.4099 0.4792 0.133 Uiso 1 1 calc R . . C30 C 0.3314(3) 0.5262(8) 0.5316(3) 0.132(3) Uani 1 1 d . . . H30A H 0.3608 0.5104 0.5435 0.158 Uiso 1 1 calc R . . H30B H 0.3286 0.5976 0.5279 0.158 Uiso 1 1 calc R . . C31 C 0.3210(3) 0.4959(9) 0.5755(3) 0.167(4) Uani 1 1 d . . . H31A H 0.2994 0.5384 0.5750 0.250 Uiso 1 1 calc R . . H31B H 0.3458 0.5012 0.6103 0.250 Uiso 1 1 calc R . . H31C H 0.3112 0.4287 0.5697 0.250 Uiso 1 1 calc R . . C32 C 0.24918(19) 0.5100(6) 0.3518(3) 0.0881(19) Uani 1 1 d . . . H32A H 0.2349 0.4804 0.3157 0.106 Uiso 1 1 calc R . . H32B H 0.2369 0.4816 0.3733 0.106 Uiso 1 1 calc R . . C33 C 0.2397(2) 0.6170(7) 0.3460(3) 0.104(2) Uani 1 1 d . . . H33A H 0.2549 0.6486 0.3290 0.124 Uiso 1 1 calc R . . H33B H 0.2494 0.6460 0.3819 0.124 Uiso 1 1 calc R . . C34 C 0.1925(3) 0.6368(8) 0.3116(3) 0.124(3) Uani 1 1 d . . . H34A H 0.1826 0.6028 0.2769 0.149 Uiso 1 1 calc R . . H34B H 0.1778 0.6087 0.3301 0.149 Uiso 1 1 calc R . . C35 C 0.1810(3) 0.7432(8) 0.3007(4) 0.151(4) Uani 1 1 d . . . H35A H 0.1874 0.7761 0.3343 0.227 Uiso 1 1 calc R . . H35B H 0.1514 0.7491 0.2760 0.227 Uiso 1 1 calc R . . H35C H 0.1970 0.7730 0.2846 0.227 Uiso 1 1 calc R . . C40 C 0.2945(2) 0.3685(7) 0.3752(3) 0.102(2) Uani 1 1 d . . . H40A H 0.2791 0.3491 0.3371 0.122 Uiso 1 1 calc R . . H40B H 0.2786 0.3450 0.3932 0.122 Uiso 1 1 calc R . . C41 C 0.3361(3) 0.3154(9) 0.3999(4) 0.145(3) Uani 1 1 d . . . H41A H 0.3516 0.3302 0.4386 0.174 Uiso 1 1 calc R . . H41B H 0.3529 0.3378 0.3827 0.174 Uiso 1 1 calc R . . C42 C 0.3285(4) 0.1986(11) 0.3912(5) 0.182(5) Uani 1 1 d . . . H42A H 0.3538 0.1637 0.4163 0.219 Uiso 1 1 calc R . . H42B H 0.3058 0.1793 0.3990 0.219 Uiso 1 1 calc R . . C36 C 0.31751(19) 0.5215(6) 0.3471(2) 0.097(2) Uani 1 1 d . . . H36A H 0.3189 0.5928 0.3514 0.117 Uiso 1 1 calc R . . H36B H 0.3463 0.4968 0.3642 0.117 Uiso 1 1 calc R . . C37 C 0.2973(2) 0.4977(6) 0.2867(3) 0.108(2) Uani 1 1 d . . . H37A H 0.2981 0.4267 0.2820 0.130 Uiso 1 1 calc R . . H37B H 0.2680 0.5179 0.2696 0.130 Uiso 1 1 calc R . . C38 C 0.3188(3) 0.5477(7) 0.2589(3) 0.118(3) Uani 1 1 d . . . H38A H 0.3479 0.5253 0.2754 0.142 Uiso 1 1 calc R . . H38B H 0.3192 0.6183 0.2655 0.142 Uiso 1 1 calc R . . C39 C 0.2995(3) 0.5312(8) 0.1987(3) 0.151(4) Uani 1 1 d . . . H39A H 0.3089 0.4688 0.1917 0.226 Uiso 1 1 calc R . . H39B H 0.3079 0.5834 0.1824 0.226 Uiso 1 1 calc R . . H39C H 0.2693 0.5308 0.1834 0.226 Uiso 1 1 calc R . . C43 C 0.3180(4) 0.1727(10) 0.3370(6) 0.215(6) Uani 1 1 d . . . H43A H 0.2891 0.1894 0.3133 0.322 Uiso 1 1 calc R . . H43B H 0.3220 0.1028 0.3350 0.322 Uiso 1 1 calc R . . H43C H 0.3359 0.2082 0.3258 0.322 Uiso 1 1 calc R . . S4 S 0.04106(8) 0.7595(2) 0.32659(9) 0.1410(10) Uani 1 1 d . . . O7 O 0.05688(19) 0.7738(4) 0.3860(2) 0.137(2) Uani 1 1 d . . . C45 C 0.0620(4) 0.6476(9) 0.3190(4) 0.194(5) Uani 1 1 d . . . H45A H 0.0521 0.5948 0.3332 0.292 Uiso 1 1 calc R . . H45B H 0.0922 0.6504 0.3386 0.292 Uiso 1 1 calc R . . H45C H 0.0532 0.6361 0.2810 0.292 Uiso 1 1 calc R . . C44 C 0.0713(4) 0.8342(8) 0.3074(4) 0.177(4) Uani 1 1 d . . . H44A H 0.1007 0.8233 0.3316 0.265 Uiso 1 1 calc R . . H44B H 0.0645 0.9024 0.3092 0.265 Uiso 1 1 calc R . . H44C H 0.0654 0.8183 0.2707 0.265 Uiso 1 1 calc R . . F1 F 0.06188(9) 0.2485(2) 0.09758(12) 0.0811(10) Uani 1 1 d . . . H9N H 0.1145(7) 0.284(5) 0.107(2) 0.11(2) Uiso 1 1 d D . . H6N H 0.0569(14) 0.1132(5) 0.0835(18) 0.045(15) Uiso 1 1 d D . . H5N H 0.0478(18) 0.1439(18) 0.144(2) 0.08(2) Uiso 1 1 d D . . H8N H 0.1112(17) 0.269(4) 0.179(2) 0.062(17) Uiso 1 1 d . . . S5 S 0.18014(18) 0.3316(4) 0.4224(2) 0.260(2) Uiso 1 1 d D . . O8 O 0.2188(3) 0.3224(8) 0.4158(4) 0.223(3) Uiso 1 1 d . . . C47 C 0.1488(4) 0.4355(8) 0.3942(6) 0.258(7) Uiso 1 1 d D . . H47A H 0.1563 0.4661 0.3686 0.387 Uiso 1 1 calc R . . H47B H 0.1531 0.4817 0.4226 0.387 Uiso 1 1 calc R . . H47C H 0.1196 0.4162 0.3756 0.387 Uiso 1 1 calc R . . C46 C 0.1923(6) 0.3528(17) 0.4901(3) 0.343(11) Uiso 1 1 d D . . H46A H 0.2218 0.3412 0.5132 0.514 Uiso 1 1 calc R . . H46B H 0.1761 0.3089 0.5003 0.514 Uiso 1 1 calc R . . H46C H 0.1856 0.4201 0.4942 0.514 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 S3 0.0824(13) 0.226(3) 0.0798(12) -0.0309(14) 0.0398(10) -0.0452(14) S1 0.1045(15) 0.168(2) 0.1388(18) 0.0002(15) 0.0733(14) 0.0359(15) S2 0.162(2) 0.1108(19) 0.1073(15) 0.0181(13) 0.0614(15) -0.0102(15) O1 0.239(9) 0.224(9) 0.092(4) -0.002(5) 0.073(5) 0.007(7) O2 0.154(6) 0.203(8) 0.100(5) 0.033(5) 0.016(4) -0.013(5) O3 0.199(6) 0.158(6) 0.123(5) -0.046(4) 0.100(5) -0.060(5) O4 0.278(10) 0.133(6) 0.151(6) -0.035(5) 0.113(6) -0.015(7) O5 0.202(7) 0.336(12) 0.114(5) -0.042(6) 0.110(6) -0.078(7) O6 0.165(6) 0.268(9) 0.147(5) 0.023(5) 0.110(5) -0.030(6) N1 0.100(4) 0.120(5) 0.072(3) 0.002(3) 0.059(3) -0.002(3) N2 0.080(4) 0.142(5) 0.080(4) 0.008(3) 0.050(3) 0.016(3) N3 0.065(3) 0.103(4) 0.083(4) 0.002(3) 0.036(3) 0.006(3) N4 0.163(8) 0.143(8) 0.086(6) 0.009(5) 0.049(6) -0.032(6) N5 0.097(4) 0.110(6) 0.081(4) 0.013(4) 0.050(3) -0.007(4) N6 0.080(3) 0.082(5) 0.086(4) 0.001(4) 0.040(3) -0.010(3) N7 0.124(5) 0.115(7) 0.116(6) -0.028(6) 0.063(5) -0.031(5) N8 0.065(4) 0.135(5) 0.067(3) -0.011(3) 0.035(3) -0.011(3) N9 0.063(3) 0.118(5) 0.063(3) -0.006(3) 0.034(3) -0.008(3) N10 0.123(6) 0.177(8) 0.107(6) 0.014(5) 0.070(5) -0.026(5) C1 0.107(6) 0.153(8) 0.081(5) -0.013(5) 0.060(5) -0.001(5) C2 0.111(6) 0.148(7) 0.103(5) 0.004(5) 0.073(5) 0.016(5) C3 0.077(4) 0.109(6) 0.097(5) -0.002(4) 0.057(4) 0.000(4) C4 0.063(4) 0.076(5) 0.090(5) -0.007(4) 0.035(4) -0.015(3) C5 0.090(5) 0.092(5) 0.085(5) 0.007(4) 0.044(4) 0.009(4) C6 0.117(6) 0.085(6) 0.100(6) -0.009(4) 0.052(5) -0.005(5) C7 0.103(6) 0.110(7) 0.084(5) -0.004(5) 0.035(5) -0.022(5) C8 0.089(5) 0.103(6) 0.098(6) 0.018(5) 0.030(5) 0.004(4) C9 0.074(4) 0.096(6) 0.098(5) -0.001(4) 0.037(4) 0.000(4) C10 0.110(5) 0.144(8) 0.101(5) 0.014(5) 0.077(5) -0.007(5) C11 0.110(5) 0.140(8) 0.084(5) 0.018(5) 0.054(4) -0.018(5) C12 0.080(4) 0.117(7) 0.072(4) 0.011(4) 0.036(4) -0.007(4) C13 0.056(4) 0.086(6) 0.085(5) -0.008(4) 0.030(3) -0.015(3) C14 0.077(4) 0.090(5) 0.084(4) -0.008(4) 0.038(4) -0.010(4) C15 0.085(5) 0.089(6) 0.099(5) -0.006(4) 0.049(4) -0.014(4) C16 0.069(4) 0.130(8) 0.082(5) -0.024(5) 0.034(4) -0.024(4) C17 0.103(6) 0.097(6) 0.100(6) -0.024(5) 0.036(5) -0.031(4) C18 0.078(4) 0.105(7) 0.087(5) -0.002(5) 0.028(4) -0.024(4) C19 0.079(5) 0.165(8) 0.063(4) 0.005(4) 0.033(4) 0.001(4) C20 0.084(4) 0.150(7) 0.071(4) -0.007(4) 0.046(4) -0.002(4) C21 0.067(4) 0.099(5) 0.077(4) 0.000(3) 0.041(3) -0.001(3) C22 0.064(4) 0.096(5) 0.070(4) -0.002(3) 0.035(3) -0.005(3) C23 0.074(4) 0.142(7) 0.081(5) -0.008(4) 0.041(4) -0.023(4) C24 0.104(6) 0.159(8) 0.073(4) -0.007(4) 0.051(4) -0.022(5) C25 0.111(6) 0.126(7) 0.081(5) 0.007(4) 0.064(5) -0.013(5) C26 0.097(5) 0.168(8) 0.097(6) 0.008(5) 0.064(5) -0.029(5) C27 0.082(5) 0.169(8) 0.075(4) 0.007(4) 0.037(4) -0.030(5) N11 0.064(3) 0.116(5) 0.074(3) -0.010(3) 0.035(3) -0.008(3) C28 0.077(4) 0.145(7) 0.075(4) -0.014(4) 0.032(4) -0.012(4) C29 0.110(5) 0.152(8) 0.083(5) -0.008(5) 0.056(4) -0.005(5) C30 0.119(6) 0.195(10) 0.084(5) -0.022(5) 0.050(5) -0.029(6) C31 0.178(9) 0.246(13) 0.101(6) -0.009(7) 0.085(7) -0.014(8) C32 0.076(4) 0.113(6) 0.083(4) -0.001(4) 0.043(4) -0.007(4) C33 0.097(6) 0.130(8) 0.096(5) -0.007(5) 0.055(4) -0.002(5) C34 0.106(6) 0.159(10) 0.116(6) 0.016(6) 0.058(5) 0.013(6) C35 0.161(9) 0.157(10) 0.162(9) 0.040(7) 0.098(7) 0.047(7) C40 0.091(5) 0.128(8) 0.089(5) -0.005(5) 0.044(4) -0.002(5) C41 0.113(7) 0.179(11) 0.128(7) -0.034(7) 0.044(6) 0.021(7) C42 0.207(12) 0.216(14) 0.135(9) 0.015(9) 0.089(9) 0.092(10) C36 0.078(4) 0.142(7) 0.087(4) -0.029(4) 0.051(4) -0.027(4) C37 0.104(5) 0.136(7) 0.097(5) -0.015(5) 0.058(4) -0.035(5) C38 0.122(6) 0.153(8) 0.106(6) -0.020(5) 0.075(5) -0.033(5) C39 0.182(9) 0.194(10) 0.100(6) -0.030(6) 0.087(6) -0.070(7) C43 0.238(14) 0.204(14) 0.202(13) 0.001(10) 0.102(11) 0.085(11) S4 0.147(2) 0.179(3) 0.0939(15) 0.0046(15) 0.0541(15) 0.0031(18) O7 0.173(5) 0.151(5) 0.089(3) 0.006(3) 0.063(3) 0.036(4) C45 0.317(16) 0.157(11) 0.145(9) -0.019(7) 0.138(10) -0.001(10) C44 0.229(12) 0.170(10) 0.143(8) 0.018(7) 0.097(9) -0.028(9) F1 0.0642(19) 0.107(3) 0.077(2) 0.0060(18) 0.0376(17) 0.0005(17) _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 1.658(6) . ? S1 C3 1.660(7) . ? S2 C12 1.657(8) . ? O1 N4 1.241(10) . ? O2 N4 1.216(10) . ? O3 N7 1.216(9) . ? O4 N7 1.193(9) . ? O5 N10 1.177(9) . ? O6 N10 1.205(8) . ? N1 C19 1.455(8) . ? N1 C10 1.468(8) . ? N1 C1 1.475(9) . ? N2 C3 1.332(8) . ? N2 C2 1.465(7) . ? N2 H2N 0.8600 . ? N3 C3 1.372(7) . ? N3 C4 1.395(8) . ? N3 H3N 0.8600 . ? N4 C7 1.454(10) . ? N5 C12 1.340(9) . ? N5 C11 1.457(8) . ? N5 H5N 0.9100(12) . ? N6 C13 1.371(8) . ? N6 C12 1.373(8) . ? N6 H6N 0.9100(11) . ? N7 C16 1.456(10) . ? N8 C21 1.354(7) . ? N8 C20 1.446(7) . ? N8 H8N 0.85(5) . ? N9 C21 1.367(7) . ? N9 C22 1.390(7) . ? N9 H9N 0.9100(11) . ? N10 C25 1.463(9) . ? C1 C2 1.524(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C4 C5 1.362(8) . ? C4 C9 1.402(9) . ? C5 C6 1.359(9) . ? C5 H5 0.9300 . ? C6 C7 1.371(10) . ? C6 H6 0.9300 . ? C7 C8 1.384(10) . ? C8 C9 1.361(9) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.497(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C13 C14 1.383(8) . ? C13 C18 1.386(9) . ? C14 C15 1.368(9) . ? C14 H14 0.9300 . ? C15 C16 1.352(10) . ? C15 H15 0.9300 . ? C16 C17 1.374(10) . ? C17 C18 1.370(10) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.519(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C22 C23 1.373(8) . ? C22 C27 1.395(8) . ? C23 C24 1.375(8) . ? C23 H23 0.9300 . ? C24 C25 1.371(9) . ? C24 H24 0.9300 . ? C25 C26 1.351(9) . ? C26 C27 1.381(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? N11 C40 1.498(9) . ? N11 C32 1.517(8) . ? N11 C36 1.518(7) . ? N11 C28 1.527(8) . ? C28 C29 1.510(9) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.496(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.485(10) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.477(10) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.528(10) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.487(11) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C40 C41 1.501(10) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.600(16) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.411(13) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C36 C37 1.516(8) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.481(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.493(10) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? S4 O7 1.482(5) . ? S4 C44 1.736(10) . ? S4 C45 1.744(11) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? S5 O8 1.484(9) . ? S5 C47 1.7393(11) . ? S5 C46 1.7396(11) . ? C47 H47A 0.9601 . ? C47 H47B 0.9601 . ? C47 H47C 0.9601 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 N1 C10 111.7(6) . . ? C19 N1 C1 110.0(6) . . ? C10 N1 C1 111.2(6) . . ? C3 N2 C2 124.5(5) . . ? C3 N2 H2N 117.8 . . ? C2 N2 H2N 117.8 . . ? C3 N3 C4 133.9(6) . . ? C3 N3 H3N 113.1 . . ? C4 N3 H3N 113.1 . . ? O2 N4 O1 122.7(9) . . ? O2 N4 C7 120.7(10) . . ? O1 N4 C7 116.0(10) . . ? C12 N5 C11 125.0(7) . . ? C12 N5 H5N 115(4) . . ? C11 N5 H5N 120(4) . . ? C13 N6 C12 133.6(7) . . ? C13 N6 H6N 116(3) . . ? C12 N6 H6N 111(3) . . ? O4 N7 O3 122.5(9) . . ? O4 N7 C16 118.5(9) . . ? O3 N7 C16 119.0(9) . . ? C21 N8 C20 125.0(6) . . ? C21 N8 H8N 116(3) . . ? C20 N8 H8N 119(3) . . ? C21 N9 C22 130.7(5) . . ? C21 N9 H9N 119(4) . . ? C22 N9 H9N 110(4) . . ? O5 N10 O6 122.7(8) . . ? O5 N10 C25 118.9(8) . . ? O6 N10 C25 118.4(8) . . ? N1 C1 C2 113.2(6) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? N2 C2 C1 109.9(5) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 N3 111.0(5) . . ? N2 C3 S1 123.4(5) . . ? N3 C3 S1 125.6(6) . . ? C5 C4 N3 116.9(6) . . ? C5 C4 C9 117.7(6) . . ? N3 C4 C9 125.4(6) . . ? C6 C5 C4 123.7(7) . . ? C6 C5 H5 118.2 . . ? C4 C5 H5 118.1 . . ? C5 C6 C7 117.6(7) . . ? C5 C6 H6 121.2 . . ? C7 C6 H6 121.2 . . ? C6 C7 C8 121.1(7) . . ? C6 C7 N4 121.2(9) . . ? C8 C7 N4 117.8(9) . . ? C9 C8 C7 120.0(7) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C4 119.9(7) . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? N1 C10 C11 112.6(5) . . ? N1 C10 H10A 109.0 . . ? C11 C10 H10A 109.1 . . ? N1 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? N5 C11 C10 111.1(6) . . ? N5 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? N5 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N5 C12 N6 111.3(7) . . ? N5 C12 S2 122.3(5) . . ? N6 C12 S2 126.4(6) . . ? N6 C13 C14 116.8(7) . . ? N6 C13 C18 126.6(7) . . ? C14 C13 C18 116.6(6) . . ? C15 C14 C13 124.4(7) . . ? C15 C14 H14 117.8 . . ? C13 C14 H14 117.8 . . ? C16 C15 C14 116.8(7) . . ? C16 C15 H15 121.6 . . ? C14 C15 H15 121.6 . . ? C15 C16 C17 121.8(7) . . ? C15 C16 N7 120.0(8) . . ? C17 C16 N7 118.1(9) . . ? C18 C17 C16 120.3(8) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C13 120.2(7) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? N1 C19 C20 114.7(6) . . ? N1 C19 H19A 108.7 . . ? C20 C19 H19A 108.6 . . ? N1 C19 H19B 108.6 . . ? C20 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? N8 C20 C19 108.1(5) . . ? N8 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? N8 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? N8 C21 N9 112.2(5) . . ? N8 C21 S3 121.0(5) . . ? N9 C21 S3 126.8(4) . . ? C23 C22 N9 116.0(5) . . ? C23 C22 C27 117.8(5) . . ? N9 C22 C27 126.2(6) . . ? C22 C23 C24 123.2(6) . . ? C22 C23 H23 118.4 . . ? C24 C23 H23 118.4 . . ? C25 C24 C23 117.7(7) . . ? C25 C24 H24 121.2 . . ? C23 C24 H24 121.1 . . ? C26 C25 C24 120.8(6) . . ? C26 C25 N10 119.8(7) . . ? C24 C25 N10 119.4(7) . . ? C25 C26 C27 121.7(6) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C26 C27 C22 118.8(6) . . ? C26 C27 H27 120.6 . . ? C22 C27 H27 120.6 . . ? C40 N11 C32 105.2(5) . . ? C40 N11 C36 110.7(5) . . ? C32 N11 C36 112.0(5) . . ? C40 N11 C28 111.9(5) . . ? C32 N11 C28 111.8(5) . . ? C36 N11 C28 105.4(5) . . ? C29 C28 N11 116.6(6) . . ? C29 C28 H28A 108.2 . . ? N11 C28 H28A 108.1 . . ? C29 C28 H28B 108.1 . . ? N11 C28 H28B 108.2 . . ? H28A C28 H28B 107.3 . . ? C30 C29 C28 111.6(6) . . ? C30 C29 H29A 109.3 . . ? C28 C29 H29A 109.3 . . ? C30 C29 H29B 109.3 . . ? C28 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? C31 C30 C29 117.2(7) . . ? C31 C30 H30A 108.1 . . ? C29 C30 H30A 108.0 . . ? C31 C30 H30B 107.9 . . ? C29 C30 H30B 108.0 . . ? H30A C30 H30B 107.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.4 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 N11 117.6(6) . . ? C33 C32 H32A 107.9 . . ? N11 C32 H32A 107.9 . . ? C33 C32 H32B 107.9 . . ? N11 C32 H32B 107.9 . . ? H32A C32 H32B 107.2 . . ? C32 C33 C34 111.7(7) . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? C34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C33 114.6(8) . . ? C35 C34 H34A 108.6 . . ? C33 C34 H34A 108.6 . . ? C35 C34 H34B 108.6 . . ? C33 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? C34 C35 H35A 109.4 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N11 C40 C41 117.8(7) . . ? N11 C40 H40A 107.8 . . ? C41 C40 H40A 107.9 . . ? N11 C40 H40B 107.9 . . ? C41 C40 H40B 107.9 . . ? H40A C40 H40B 107.2 . . ? C40 C41 C42 109.8(8) . . ? C40 C41 H41A 109.7 . . ? C42 C41 H41A 109.7 . . ? C40 C41 H41B 109.7 . . ? C42 C41 H41B 109.6 . . ? H41A C41 H41B 108.2 . . ? C43 C42 C41 110.2(11) . . ? C43 C42 H42A 109.6 . . ? C41 C42 H42A 109.6 . . ? C43 C42 H42B 109.6 . . ? C41 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? C37 C36 N11 115.5(5) . . ? C37 C36 H36A 108.4 . . ? N11 C36 H36A 108.4 . . ? C37 C36 H36B 108.4 . . ? N11 C36 H36B 108.4 . . ? H36A C36 H36B 107.5 . . ? C38 C37 C36 112.4(6) . . ? C38 C37 H37A 109.1 . . ? C36 C37 H37A 109.1 . . ? C38 C37 H37B 109.1 . . ? C36 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? C37 C38 C39 115.5(6) . . ? C37 C38 H38A 108.4 . . ? C39 C38 H38A 108.4 . . ? C37 C38 H38B 108.4 . . ? C39 C38 H38B 108.4 . . ? H38A C38 H38B 107.5 . . ? C38 C39 H39A 109.4 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O7 S4 C44 107.2(4) . . ? O7 S4 C45 106.5(4) . . ? C44 S4 C45 95.9(6) . . ? S4 C45 H45A 109.5 . . ? S4 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? S4 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? S4 C44 H44A 109.5 . . ? S4 C44 H44B 109.4 . . ? H44A C44 H44B 109.5 . . ? S4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O8 S5 C47 117.1(7) . . ? O8 S5 C46 111.7(8) . . ? C47 S5 C46 97.8(9) . . ? S5 C47 H47A 109.5 . . ? S5 C47 H47B 109.4 . . ? H47A C47 H47B 109.5 . . ? S5 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? S5 C46 H46A 110.0 . . ? S5 C46 H46B 110.0 . . ? H46A C46 H46B 109.0 . . ? S5 C46 H46C 109.0 . . ? H46A C46 H46C 110.0 . . ? H46B C46 H46C 109.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 N1 C1 C2 165.3(5) . . . . ? C10 N1 C1 C2 -70.4(7) . . . . ? C3 N2 C2 C1 -172.4(7) . . . . ? N1 C1 C2 N2 -51.4(8) . . . . ? C2 N2 C3 N3 -172.3(6) . . . . ? C2 N2 C3 S1 6.6(10) . . . . ? C4 N3 C3 N2 -176.8(6) . . . . ? C4 N3 C3 S1 4.3(11) . . . . ? C3 N3 C4 C5 -177.3(6) . . . . ? C3 N3 C4 C9 5.9(11) . . . . ? N3 C4 C5 C6 -179.5(6) . . . . ? C9 C4 C5 C6 -2.3(10) . . . . ? C4 C5 C6 C7 1.8(11) . . . . ? C5 C6 C7 C8 -0.5(11) . . . . ? C5 C6 C7 N4 -178.9(7) . . . . ? O2 N4 C7 C6 -179.3(9) . . . . ? O1 N4 C7 C6 -7.8(12) . . . . ? O2 N4 C7 C8 2.3(12) . . . . ? O1 N4 C7 C8 173.8(8) . . . . ? C6 C7 C8 C9 0.0(11) . . . . ? N4 C7 C8 C9 178.4(6) . . . . ? C7 C8 C9 C4 -0.6(10) . . . . ? C5 C4 C9 C8 1.7(9) . . . . ? N3 C4 C9 C8 178.5(6) . . . . ? C19 N1 C10 C11 -69.1(7) . . . . ? C1 N1 C10 C11 167.6(6) . . . . ? C12 N5 C11 C10 -178.3(6) . . . . ? N1 C10 C11 N5 -50.9(8) . . . . ? C11 N5 C12 N6 -176.7(6) . . . . ? C11 N5 C12 S2 2.9(10) . . . . ? C13 N6 C12 N5 -172.2(6) . . . . ? C13 N6 C12 S2 8.2(10) . . . . ? C12 N6 C13 C14 179.9(6) . . . . ? C12 N6 C13 C18 1.3(11) . . . . ? N6 C13 C14 C15 178.8(5) . . . . ? C18 C13 C14 C15 -2.5(9) . . . . ? C13 C14 C15 C16 1.0(9) . . . . ? C14 C15 C16 C17 0.5(10) . . . . ? C14 C15 C16 N7 -179.1(6) . . . . ? O4 N7 C16 C15 179.9(8) . . . . ? O3 N7 C16 C15 -2.0(11) . . . . ? O4 N7 C16 C17 0.2(11) . . . . ? O3 N7 C16 C17 178.3(7) . . . . ? C15 C16 C17 C18 -0.4(11) . . . . ? N7 C16 C17 C18 179.3(6) . . . . ? C16 C17 C18 C13 -1.2(10) . . . . ? N6 C13 C18 C17 -178.9(6) . . . . ? C14 C13 C18 C17 2.5(9) . . . . ? C10 N1 C19 C20 163.5(6) . . . . ? C1 N1 C19 C20 -72.5(7) . . . . ? C21 N8 C20 C19 -159.3(7) . . . . ? N1 C19 C20 N8 -49.3(8) . . . . ? C20 N8 C21 N9 -173.1(6) . . . . ? C20 N8 C21 S3 9.1(10) . . . . ? C22 N9 C21 N8 -176.9(6) . . . . ? C22 N9 C21 S3 0.7(11) . . . . ? C21 N9 C22 C23 174.8(7) . . . . ? C21 N9 C22 C27 -4.7(12) . . . . ? N9 C22 C23 C24 -177.1(7) . . . . ? C27 C22 C23 C24 2.4(11) . . . . ? C22 C23 C24 C25 -0.8(12) . . . . ? C23 C24 C25 C26 -0.8(12) . . . . ? C23 C24 C25 N10 177.6(7) . . . . ? O5 N10 C25 C26 172.2(10) . . . . ? O6 N10 C25 C26 -8.6(13) . . . . ? O5 N10 C25 C24 -6.2(14) . . . . ? O6 N10 C25 C24 173.0(9) . . . . ? C24 C25 C26 C27 0.7(13) . . . . ? N10 C25 C26 C27 -177.7(7) . . . . ? C25 C26 C27 C22 0.9(12) . . . . ? C23 C22 C27 C26 -2.4(11) . . . . ? N9 C22 C27 C26 177.0(7) . . . . ? C40 N11 C28 C29 -56.3(8) . . . . ? C32 N11 C28 C29 61.4(9) . . . . ? C36 N11 C28 C29 -176.6(6) . . . . ? N11 C28 C29 C30 -178.2(6) . . . . ? C28 C29 C30 C31 -179.3(8) . . . . ? C40 N11 C32 C33 -177.3(5) . . . . ? C36 N11 C32 C33 -57.0(7) . . . . ? C28 N11 C32 C33 61.1(7) . . . . ? N11 C32 C33 C34 171.0(5) . . . . ? C32 C33 C34 C35 -175.7(7) . . . . ? C32 N11 C40 C41 -177.8(6) . . . . ? C36 N11 C40 C41 61.0(8) . . . . ? C28 N11 C40 C41 -56.3(8) . . . . ? N11 C40 C41 C42 -178.0(6) . . . . ? C40 C41 C42 C43 77.1(11) . . . . ? C40 N11 C36 C37 61.6(8) . . . . ? C32 N11 C36 C37 -55.4(9) . . . . ? C28 N11 C36 C37 -177.2(6) . . . . ? N11 C36 C37 C38 175.5(7) . . . . ? C36 C37 C38 C39 -177.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.624 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.054