# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5b_MeCN _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H50 N2 O2 S4, C2 H3 N' _chemical_formula_sum 'C42 H53 N3 O2 S4' _chemical_formula_weight 757.09 # start Validation Reply Form _vrf_PLAT021_13diam ; PROBLEM: Ratio Unique / Expected Reflections too High ... 6.488 RESPONSE: SHELXL HKLF 5 Refinement ; # end Validation Reply Form 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 Orthorhombic _symmetry_space_group_name_H-M 'P c c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 15.400(5) _cell_length_b 15.405(5) _cell_length_c 17.403(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4129(2) _cell_formula_units_Z 4 _cell_measurement_temperature 113 _cell_measurement_reflns_used 9344 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 0.268 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8728 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 113 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 27.48 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30747 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.49 _reflns_number_total 30747 _reflns_number_gt 21020 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FS-PROCESS-AUTO(Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'FS-PROCESS-AUTO(Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996) and PLATON (Spek, 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita, 2001, Kabuto et al., 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0843P)^2^+9.1652P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 30747 _refine_ls_number_parameters 455 _refine_ls_number_restraints 736 _refine_ls_R_factor_all 0.1383 _refine_ls_R_factor_gt 0.0974 _refine_ls_wR_factor_ref 0.2325 _refine_ls_wR_factor_gt 0.2057 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S2B S 0.0605(4) 0.4107(4) 0.3604(2) 0.0419(7) Uani 0.50 1 d PU . 2 S2A S 0.0898(6) 0.0495(4) 0.3460(6) 0.0370(9) Uani 0.50 1 d PU A 1 S1B S 0.0802(6) 0.0669(5) 0.3551(6) 0.0412(10) Uani 0.50 1 d PU B 2 S1A S 0.0546(4) 0.4222(4) 0.3410(2) 0.0378(7) Uani 0.50 1 d PU . 1 O1A O 0.1173(4) 0.2504(3) 0.4081(4) 0.0352(10) Uani 0.50 1 d PDU A 1 C1A C 0.0689(4) 0.2418(7) 0.3374(4) 0.0377(7) Uani 0.50 1 d PDU A 1 C2A C 0.0385(5) 0.3136(9) 0.3000(5) 0.0377(7) Uani 0.50 1 d PDU A 1 C3A C -0.0068(5) 0.3072(6) 0.2367(5) 0.0416(7) Uani 0.50 1 d PDU A 1 H3A H -0.0296 0.3582 0.2137 0.050 Uiso 0.50 1 calc PR A 1 C4A C -0.0224(4) 0.2266(4) 0.2025(3) 0.0454(6) Uani 0.50 1 d PDU A 1 C5A C 0.0064(4) 0.1526(5) 0.2435(3) 0.0431(7) Uani 0.50 1 d PDU A 1 H5A H -0.0060 0.0966 0.2235 0.052 Uiso 0.50 1 calc PR A 1 C6A C 0.0488(5) 0.1588(9) 0.3067(6) 0.0397(7) Uani 0.50 1 d PDU A 1 C7A C -0.0683(4) 0.2179(4) 0.1260(3) 0.0514(7) Uani 0.50 1 d PDU A 1 C8A C -0.0738(4) 0.3047(4) 0.0828(4) 0.0579(11) Uani 0.50 1 d PDU A 1 H8A H -0.0948 0.2945 0.0304 0.087 Uiso 0.50 1 calc PR A 1 H8A0 H -0.0161 0.3315 0.0808 0.087 Uiso 0.50 1 calc PR A 1 H8A1 H -0.1141 0.3436 0.1096 0.087 Uiso 0.50 1 calc PR A 1 C9A C -0.1481(4) 0.1706(5) 0.1295(4) 0.0593(13) Uani 0.50 1 d PDU A 1 H9A H -0.1901 0.2028 0.1607 0.089 Uiso 0.50 1 calc PR A 1 H9A0 H -0.1376 0.1136 0.1528 0.089 Uiso 0.50 1 calc PR A 1 H9A1 H -0.1711 0.1628 0.0775 0.089 Uiso 0.50 1 calc PR A 1 C10A C -0.0275(5) 0.1488(5) 0.0649(5) 0.0557(13) Uani 0.50 1 d PDU A 1 H10A H -0.0456 0.1645 0.0127 0.084 Uiso 0.50 1 calc PR A 1 H10B H -0.0484 0.0903 0.0770 0.084 Uiso 0.50 1 calc PR A 1 H10C H 0.0360 0.1501 0.0682 0.084 Uiso 0.50 1 calc PR A 1 O1B O 0.2607(4) 0.1279(3) 0.4071(3) 0.0383(10) Uani 0.50 1 d PDU B 2 C1B C 0.2667(7) 0.0737(4) 0.3372(4) 0.0437(7) Uani 0.50 1 d PDU B 2 C2B C 0.1902(11) 0.0432(6) 0.3070(7) 0.0444(7) Uani 0.50 1 d PDU B 2 C3B C 0.1924(5) -0.0043(5) 0.2469(4) 0.0484(7) Uani 0.50 1 d PDU B 2 H3B H 0.1389 -0.0267 0.2282 0.058 Uiso 0.50 1 calc PR B 2 C4B C 0.2670(4) -0.0256(4) 0.2072(3) 0.0514(7) Uani 0.50 1 d PDU B 2 C5B C 0.3455(5) 0.0035(4) 0.2408(4) 0.0490(7) Uani 0.50 1 d PDU B 2 H5B H 0.3994 -0.0123 0.2182 0.059 Uiso 0.50 1 calc PR B 2 C6B C 0.3447(9) 0.0511(6) 0.3015(6) 0.0452(7) Uani 0.50 1 d PDU . 2 C7B C 0.2723(4) -0.0806(4) 0.1352(4) 0.0610(8) Uani 0.50 1 d PDU B 2 C8B C 0.1886(4) -0.1168(4) 0.1044(4) 0.0692(12) Uani 0.50 1 d PDU B 2 H8B H 0.1472 -0.0694 0.0961 0.104 Uiso 0.50 1 calc PR B 2 H8B0 H 0.1643 -0.1581 0.1415 0.104 Uiso 0.50 1 calc PR B 2 H8B1 H 0.1996 -0.1466 0.0556 0.104 Uiso 0.50 1 calc PR B 2 C9B C 0.3313(5) -0.0428(5) 0.0794(4) 0.0697(12) Uani 0.50 1 d PDU B 2 H9B H 0.3229 -0.0709 0.0294 0.104 Uiso 0.50 1 calc PR B 2 H9B0 H 0.3913 -0.0514 0.0965 0.104 Uiso 0.50 1 calc PR B 2 H9B1 H 0.3195 0.0195 0.0747 0.104 Uiso 0.50 1 calc PR B 2 C10B C 0.3263(5) -0.1723(5) 0.1478(4) 0.0730(14) Uani 0.50 1 d PDU B 2 H10D H 0.2960 -0.2082 0.1858 0.110 Uiso 0.50 1 calc PR B 2 H10E H 0.3850 -0.1594 0.1662 0.110 Uiso 0.50 1 calc PR B 2 H10F H 0.3297 -0.2037 0.0989 0.110 Uiso 0.50 1 calc PR B 2 N1A N 0.2547(5) 0.0958(4) 0.4185(4) 0.0526(12) Uani 0.50 1 d PDU A 1 C11A C 0.2605(7) 0.0652(3) 0.3473(5) 0.0424(7) Uani 0.50 1 d PDU A 1 C12A C 0.1856(11) 0.0379(6) 0.3047(7) 0.0442(7) Uani 0.50 1 d PDU A 1 C13A C 0.1939(6) 0.0057(5) 0.2256(4) 0.0484(7) Uani 0.50 1 d PDU A 1 H13A H 0.1430 -0.0108 0.1985 0.058 Uiso 0.50 1 calc PR A 1 C14A C 0.2735(4) -0.0014(4) 0.1891(4) 0.0509(7) Uani 0.50 1 d PDU A 1 C15A C 0.3459(5) 0.0249(4) 0.2305(4) 0.0487(7) Uani 0.50 1 d PDU A 1 H15A H 0.4011 0.0234 0.2063 0.058 Uiso 0.50 1 calc PR A 1 C16A C 0.3404(9) 0.0553(6) 0.3111(6) 0.0451(7) Uani 0.50 1 d PDU . 1 C17A C 0.2762(4) -0.0378(4) 0.1076(4) 0.0572(9) Uani 0.50 1 d PDU A 1 C18A C 0.1934(4) -0.0294(5) 0.0665(4) 0.0659(14) Uani 0.50 1 d PDU A 1 H18A H 0.1795 0.0322 0.0598 0.099 Uiso 0.50 1 calc PR A 1 H18B H 0.1473 -0.0576 0.0962 0.099 Uiso 0.50 1 calc PR A 1 H18C H 0.1982 -0.0573 0.0161 0.099 Uiso 0.50 1 calc PR A 1 C19A C 0.3508(5) 0.0071(5) 0.0594(5) 0.0708(15) Uani 0.50 1 d PDU A 1 H19A H 0.3392 0.0695 0.0555 0.106 Uiso 0.50 1 calc PR A 1 H19B H 0.3526 -0.0182 0.0077 0.106 Uiso 0.50 1 calc PR A 1 H19C H 0.4067 -0.0021 0.0849 0.106 Uiso 0.50 1 calc PR A 1 C20A C 0.2917(5) -0.1321(4) 0.1177(4) 0.0728(11) Uani 0.50 1 d PDU A 1 H20A H 0.2760 -0.1628 0.0704 0.109 Uiso 0.50 1 calc PR A 1 H20B H 0.2562 -0.1538 0.1603 0.109 Uiso 0.50 1 calc PR A 1 H20C H 0.3532 -0.1421 0.1291 0.109 Uiso 0.50 1 calc PR A 1 N1B N 0.1076(5) 0.2229(4) 0.4155(4) 0.0423(12) Uani 0.50 1 d PDU B 2 C11B C 0.0731(4) 0.2345(7) 0.3471(4) 0.0370(7) Uani 0.50 1 d PDU B 2 C12B C 0.0437(5) 0.3130(9) 0.3127(5) 0.0381(6) Uani 0.50 1 d PDU B 2 C13B C 0.0070(5) 0.3148(6) 0.2341(5) 0.0418(7) Uani 0.50 1 d PDU B 2 H13B H -0.0128 0.3681 0.2130 0.050 Uiso 0.50 1 calc PR B 2 C14B C 0.0012(4) 0.2388(4) 0.1907(3) 0.0444(6) Uani 0.50 1 d PDU B 2 C15B C 0.0250(4) 0.1602(4) 0.2238(3) 0.0432(7) Uani 0.50 1 d PDU B 2 H15B H 0.0189 0.1078 0.1955 0.052 Uiso 0.50 1 calc PR B 2 C16B C 0.0597(5) 0.1578(9) 0.3032(6) 0.0402(7) Uani 0.50 1 d PDU B 2 C17B C -0.0377(4) 0.2427(4) 0.1099(3) 0.0494(7) Uani 0.50 1 d PDU B 2 C18B C 0.0024(4) 0.3170(4) 0.0655(4) 0.0554(13) Uani 0.50 1 d PDU B 2 H18D H -0.0130 0.3119 0.0111 0.083 Uiso 0.50 1 calc PR B 2 H18E H 0.0657 0.3151 0.0711 0.083 Uiso 0.50 1 calc PR B 2 H18F H -0.0195 0.3722 0.0857 0.083 Uiso 0.50 1 calc PR B 2 C19B C -0.1377(4) 0.2585(4) 0.1191(4) 0.0613(11) Uani 0.50 1 d PDU B 2 H19D H -0.1633 0.2112 0.1491 0.092 Uiso 0.50 1 calc PR B 2 H19E H -0.1649 0.2606 0.0682 0.092 Uiso 0.50 1 calc PR B 2 H19F H -0.1473 0.3138 0.1457 0.092 Uiso 0.50 1 calc PR B 2 C20B C -0.0002(5) 0.1702(5) 0.0706(5) 0.0629(13) Uani 0.50 1 d PDU B 2 H20D H -0.0227 0.1161 0.0926 0.094 Uiso 0.50 1 calc PR B 2 H20E H 0.0631 0.1718 0.0764 0.094 Uiso 0.50 1 calc PR B 2 H20F H -0.0152 0.1731 0.0160 0.094 Uiso 0.50 1 calc PR B 2 C1S C 0.2500 0.2500 0.2032(2) 0.0727(9) Uiso 1 2 d SU . . N1SB N 0.2366 0.1789 0.0831 0.108(2) Uiso 0.25 1 d PU C 2 C2SB C 0.2449 0.2100 0.1404 0.0876(16) Uiso 0.25 1 d PU . 2 C2SA C 0.2500 0.2500 0.1257(5) 0.0848(14) Uiso 0.50 2 d SPU . 1 N1SA N 0.2500 0.2500 0.0592(6) 0.140(2) Uiso 0.50 2 d SPU . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S2B 0.0382(12) 0.0456(15) 0.0418(17) 0.0055(12) 0.0154(13) -0.0015(10) S2A 0.0304(18) 0.030(2) 0.051(2) 0.0070(18) 0.0086(12) 0.0037(15) S1B 0.0304(16) 0.037(2) 0.057(2) -0.0011(18) 0.0062(12) 0.0097(15) S1A 0.0333(10) 0.0433(14) 0.0367(17) 0.0095(12) 0.0024(12) 0.0032(9) O1A 0.0338(18) 0.033(2) 0.0390(19) 0.0118(17) -0.0016(16) -0.0104(17) C1A 0.0392(12) 0.0390(12) 0.0349(13) 0.0026(12) 0.0094(11) -0.0019(11) C2A 0.0407(13) 0.0371(13) 0.0352(13) 0.0015(12) 0.0093(11) -0.0013(11) C3A 0.0476(13) 0.0399(13) 0.0372(13) 0.0034(12) 0.0053(11) -0.0011(12) C4A 0.0522(13) 0.0447(12) 0.0392(12) 0.0039(11) 0.0005(11) -0.0035(11) C5A 0.0482(14) 0.0416(13) 0.0393(13) 0.0051(12) 0.0037(12) -0.0039(12) C6A 0.0428(13) 0.0392(12) 0.0370(13) 0.0045(11) 0.0062(12) -0.0032(12) C7A 0.0596(15) 0.0512(14) 0.0434(13) 0.0045(12) -0.0040(13) -0.0049(12) C8A 0.070(2) 0.055(2) 0.049(2) 0.0120(19) -0.0148(19) 0.000(2) C9A 0.068(3) 0.052(2) 0.058(3) 0.017(2) -0.025(2) -0.015(2) C10A 0.060(3) 0.061(2) 0.046(2) -0.008(2) -0.002(2) -0.012(2) O1B 0.0405(18) 0.0180(18) 0.056(2) 0.0062(17) 0.0027(16) -0.0033(17) C1B 0.0415(12) 0.0353(13) 0.0543(15) 0.0006(12) -0.0057(12) -0.0036(12) C2B 0.0412(13) 0.0381(13) 0.0540(15) 0.0017(12) -0.0041(12) -0.0033(12) C3B 0.0430(13) 0.0446(14) 0.0575(15) -0.0013(12) -0.0058(13) -0.0049(12) C4B 0.0471(12) 0.0486(14) 0.0583(15) -0.0062(12) -0.0065(12) -0.0034(12) C5B 0.0439(13) 0.0447(14) 0.0586(15) -0.0044(12) -0.0053(12) -0.0027(13) C6B 0.0412(13) 0.0379(13) 0.0564(15) -0.0023(12) -0.0058(12) -0.0020(12) C7B 0.0597(14) 0.0588(16) 0.0646(16) -0.0129(14) -0.0062(13) -0.0002(14) C8B 0.064(2) 0.073(2) 0.071(3) -0.023(2) -0.016(2) -0.002(2) C9B 0.072(2) 0.069(2) 0.069(2) -0.019(2) -0.010(2) -0.004(2) C10B 0.072(3) 0.069(3) 0.078(3) -0.008(3) -0.008(3) 0.009(3) N1A 0.048(2) 0.043(2) 0.067(2) -0.002(2) -0.012(2) -0.009(2) C11A 0.0406(12) 0.0339(13) 0.0528(15) 0.0026(12) -0.0050(12) -0.0036(12) C12A 0.0411(13) 0.0376(13) 0.0541(15) 0.0015(12) -0.0046(12) -0.0039(12) C13A 0.0445(13) 0.0441(14) 0.0567(15) -0.0017(13) -0.0055(13) -0.0052(12) C14A 0.0480(12) 0.0465(13) 0.0582(15) -0.0049(12) -0.0054(11) -0.0041(12) C15A 0.0445(13) 0.0437(14) 0.0580(15) -0.0028(13) -0.0049(12) -0.0031(13) C16A 0.0417(13) 0.0377(13) 0.0558(15) -0.0023(12) -0.0063(12) -0.0027(12) C17A 0.0565(16) 0.0544(17) 0.0607(18) -0.0117(15) -0.0027(15) -0.0024(16) C18A 0.060(3) 0.078(3) 0.060(3) -0.018(3) -0.010(2) -0.012(3) C19A 0.064(3) 0.081(3) 0.068(3) -0.013(3) 0.001(3) -0.001(3) C20A 0.076(2) 0.070(2) 0.073(2) -0.017(2) -0.012(2) 0.006(2) N1B 0.046(2) 0.039(2) 0.042(2) -0.010(2) 0.0003(19) -0.007(2) C11B 0.0393(12) 0.0378(12) 0.0339(13) 0.0041(12) 0.0113(11) -0.0015(11) C12B 0.0403(12) 0.0389(12) 0.0351(13) 0.0023(11) 0.0106(11) -0.0019(10) C13B 0.0475(13) 0.0406(13) 0.0375(12) 0.0024(11) 0.0053(11) -0.0003(12) C14B 0.0498(13) 0.0446(12) 0.0389(12) 0.0041(11) 0.0019(11) -0.0028(11) C15B 0.0476(14) 0.0430(13) 0.0390(13) 0.0029(12) 0.0047(12) -0.0031(12) C16B 0.0431(13) 0.0402(12) 0.0371(13) 0.0045(11) 0.0058(12) -0.0035(12) C17B 0.0558(15) 0.0514(14) 0.0411(13) 0.0043(12) -0.0035(13) -0.0042(12) C18B 0.068(3) 0.059(3) 0.040(2) 0.007(2) -0.010(2) -0.006(2) C19B 0.068(2) 0.060(2) 0.055(2) 0.0100(19) -0.0137(19) 0.0001(19) C20B 0.073(3) 0.068(3) 0.047(2) 0.003(2) -0.001(2) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S2B C12B 1.739(14) . ? S2B C6B 1.877(14) 2 ? S2A C12A 1.650(17) . ? S2A C6A 1.925(15) . ? S1B C16B 1.696(16) . ? S1B C2B 1.925(17) . ? S1A C16A 1.735(15) 2 ? S1A C2A 1.835(14) . ? O1A C1A 1.445(9) . ? C1A C2A 1.367(14) . ? C1A C6A 1.419(15) . ? C2A C3A 1.306(13) . ? C3A C4A 1.398(9) . ? C3A H3A 0.9500 . ? C4A C5A 1.416(7) . ? C4A C7A 1.514(7) . ? C5A C6A 1.283(11) . ? C5A H5A 0.9500 . ? C7A C9A 1.430(7) . ? C7A C8A 1.536(7) . ? C7A C10A 1.631(8) . ? C8A H8A 0.9800 . ? C8A H8A0 0.9800 . ? C8A H8A1 0.9800 . ? C9A H9A 0.9800 . ? C9A H9A0 0.9800 . ? C9A H9A1 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? O1B C1B 1.479(9) . ? C1B C2B 1.372(15) . ? C1B C6B 1.396(14) . ? C2B C3B 1.277(14) . ? C3B C4B 1.380(8) . ? C3B H3B 0.9500 . ? C4B C5B 1.415(7) . ? C4B C7B 1.515(7) . ? C5B C6B 1.287(11) . ? C5B H5B 0.9500 . ? C6B S2B 1.877(14) 2 ? C7B C9B 1.451(8) . ? C7B C8B 1.504(7) . ? C7B C10B 1.653(8) . ? C8B H8B 0.9800 . ? C8B H8B0 0.9800 . ? C8B H8B1 0.9800 . ? C9B H9B 0.9800 . ? C9B H9B0 0.9800 . ? C9B H9B1 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? N1A C11A 1.328(9) . ? C11A C16A 1.390(14) . ? C11A C12A 1.435(15) . ? C12A C13A 1.470(14) . ? C13A C14A 1.384(8) . ? C13A H13A 0.9500 . ? C14A C15A 1.387(7) . ? C14A C17A 1.526(7) . ? C15A C16A 1.480(11) . ? C15A H15A 0.9500 . ? C16A S1A 1.735(15) 2 ? C17A C18A 1.467(7) . ? C17A C20A 1.483(9) . ? C17A C19A 1.583(8) . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? N1B C11B 1.315(9) . ? C11B C12B 1.424(14) . ? C11B C16B 1.422(15) . ? C12B C13B 1.480(13) . ? C13B C14B 1.397(9) . ? C13B H13B 0.9500 . ? C14B C15B 1.390(7) . ? C14B C17B 1.530(6) . ? C15B C16B 1.482(11) . ? C15B H15B 0.9500 . ? C17B C20B 1.431(9) . ? C17B C18B 1.513(6) . ? C17B C19B 1.567(8) . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C1S C2SB 1.257(3) 2 ? C1S C2SB 1.257(3) . ? C1S C2SA 1.350(9) . ? N1SB C2SB 1.1136(3) . ? C2SB C2SB 1.2424(4) 2 ? C2SA N1SA 1.157(11) . ? 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 C12B S2B C6B 97.3(4) . 2 ? C12A S2A C6A 103.5(5) . . ? C16B S1B C2B 95.1(5) . . ? C16A S1A C2A 101.0(4) 2 . ? C2A C1A C6A 118.4(8) . . ? C2A C1A O1A 120.5(8) . . ? C6A C1A O1A 121.0(8) . . ? C3A C2A C1A 121.5(11) . . ? C3A C2A S1A 118.0(10) . . ? C1A C2A S1A 120.4(7) . . ? C2A C3A C4A 121.2(10) . . ? C2A C3A H3A 119.4 . . ? C4A C3A H3A 119.4 . . ? C3A C4A C5A 116.5(6) . . ? C3A C4A C7A 122.2(6) . . ? C5A C4A C7A 121.3(5) . . ? C6A C5A C4A 122.1(8) . . ? C6A C5A H5A 119.0 . . ? C4A C5A H5A 119.0 . . ? C5A C6A C1A 120.0(10) . . ? C5A C6A S2A 114.0(9) . . ? C1A C6A S2A 125.7(8) . . ? C9A C7A C4A 114.1(5) . . ? C9A C7A C8A 114.7(5) . . ? C4A C7A C8A 112.3(5) . . ? C9A C7A C10A 91.5(5) . . ? C4A C7A C10A 116.8(5) . . ? C8A C7A C10A 105.7(5) . . ? C2B C1B C6B 118.9(8) . . ? C2B C1B O1B 117.0(8) . . ? C6B C1B O1B 124.1(9) . . ? C3B C2B C1B 119.2(12) . . ? C3B C2B S1B 119.2(12) . . ? C1B C2B S1B 121.6(9) . . ? C2B C3B C4B 124.6(10) . . ? C2B C3B H3B 117.7 . . ? C4B C3B H3B 117.7 . . ? C3B C4B C5B 115.4(6) . . ? C3B C4B C7B 126.3(5) . . ? C5B C4B C7B 118.2(5) . . ? C6B C5B C4B 120.8(8) . . ? C6B C5B H5B 119.6 . . ? C4B C5B H5B 119.6 . . ? C5B C6B C1B 121.0(11) . . ? C5B C6B S2B 128.3(9) . 2 ? C1B C6B S2B 110.4(7) . 2 ? C9B C7B C8B 116.6(6) . . ? C9B C7B C4B 111.2(5) . . ? C8B C7B C4B 117.1(5) . . ? C9B C7B C10B 96.8(5) . . ? C8B C7B C10B 99.3(5) . . ? C4B C7B C10B 113.3(4) . . ? C7B C8B H8B 109.5 . . ? C7B C8B H8B0 109.5 . . ? H8B C8B H8B0 109.5 . . ? C7B C8B H8B1 109.5 . . ? H8B C8B H8B1 109.5 . . ? H8B0 C8B H8B1 109.5 . . ? C7B C9B H9B 109.5 . . ? C7B C9B H9B0 109.5 . . ? H9B C9B H9B0 109.5 . . ? C7B C9B H9B1 109.5 . . ? H9B C9B H9B1 109.5 . . ? H9B0 C9B H9B1 109.5 . . ? C7B C10B H10D 109.5 . . ? C7B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C7B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? N1A C11A C16A 121.5(9) . . ? N1A C11A C12A 122.1(8) . . ? C16A C11A C12A 116.4(9) . . ? C11A C12A C13A 120.9(11) . . ? C11A C12A S2A 117.5(9) . . ? C13A C12A S2A 121.5(12) . . ? C14A C13A C12A 122.2(9) . . ? C14A C13A H13A 118.9 . . ? C12A C13A H13A 118.9 . . ? C13A C14A C15A 116.8(6) . . ? C13A C14A C17A 118.6(5) . . ? C15A C14A C17A 124.6(6) . . ? C14A C15A C16A 122.6(8) . . ? C14A C15A H15A 118.7 . . ? C16A C15A H15A 118.7 . . ? C11A C16A C15A 121.0(10) . . ? C11A C16A S1A 131.8(8) . 2 ? C15A C16A S1A 107.1(7) . 2 ? C18A C17A C20A 106.5(5) . . ? C18A C17A C14A 113.4(5) . . ? C20A C17A C14A 104.8(5) . . ? C18A C17A C19A 109.5(6) . . ? C20A C17A C19A 112.0(5) . . ? C14A C17A C19A 110.6(5) . . ? N1B C11B C12B 128.6(9) . . ? N1B C11B C16B 115.7(9) . . ? C12B C11B C16B 115.6(8) . . ? C11B C12B C13B 121.8(10) . . ? C11B C12B S2B 119.1(7) . . ? C13B C12B S2B 118.8(9) . . ? C14B C13B C12B 120.5(8) . . ? C14B C13B H13B 119.7 . . ? C12B C13B H13B 119.7 . . ? C15B C14B C13B 119.3(6) . . ? C15B C14B C17B 121.2(5) . . ? C13B C14B C17B 119.3(5) . . ? C14B C15B C16B 120.2(7) . . ? C14B C15B H15B 119.9 . . ? C16B C15B H15B 119.9 . . ? C11B C16B C15B 122.2(10) . . ? C11B C16B S1B 111.9(8) . . ? C15B C16B S1B 125.7(9) . . ? C20B C17B C18B 100.5(6) . . ? C20B C17B C14B 104.5(5) . . ? C18B C17B C14B 109.8(4) . . ? C20B C17B C19B 124.6(5) . . ? C18B C17B C19B 109.6(5) . . ? C14B C17B C19B 107.3(4) . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5 . . ? C17B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C17B C20B H20D 109.5 . . ? C17B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C17B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C2SB C1S C2SB 59.21(17) 2 . ? N1SB C2SB C2SB 116.180(10) . 2 ? N1SB C2SB C1S 175.23(6) . . ? C2SB C2SB C1S 60.39(9) 2 . ? N1SA C2SA C1S 180.000(1) . . ? 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 C6A C1A C2A C3A -1.2(4) . . . . ? O1A C1A C2A C3A -178.7(3) . . . . ? C6A C1A C2A S1A 174.9(5) . . . . ? O1A C1A C2A S1A -2.6(5) . . . . ? C16A S1A C2A C3A -101.4(5) 2 . . . ? C16A S1A C2A C1A 82.4(5) 2 . . . ? C1A C2A C3A C4A -3.3(6) . . . . ? S1A C2A C3A C4A -179.5(6) . . . . ? C2A C3A C4A C5A 5.7(7) . . . . ? C2A C3A C4A C7A -174.9(4) . . . . ? C3A C4A C5A C6A -3.7(7) . . . . ? C7A C4A C5A C6A 176.9(5) . . . . ? C4A C5A C6A C1A -0.6(7) . . . . ? C4A C5A C6A S2A -174.5(5) . . . . ? C2A C1A C6A C5A 3.1(5) . . . . ? O1A C1A C6A C5A -179.4(4) . . . . ? C2A C1A C6A S2A 176.3(6) . . . . ? O1A C1A C6A S2A -6.2(7) . . . . ? C12A S2A C6A C5A 88.6(8) . . . . ? C12A S2A C6A C1A -84.9(8) . . . . ? C3A C4A C7A C9A -118.1(6) . . . . ? C5A C4A C7A C9A 61.2(7) . . . . ? C3A C4A C7A C8A 14.6(7) . . . . ? C5A C4A C7A C8A -166.0(5) . . . . ? C3A C4A C7A C10A 137.0(6) . . . . ? C5A C4A C7A C10A -43.7(7) . . . . ? C6B C1B C2B C3B -0.5(4) . . . . ? O1B C1B C2B C3B -179.6(3) . . . . ? C6B C1B C2B S1B 177.2(6) . . . . ? O1B C1B C2B S1B -1.8(6) . . . . ? C16B S1B C2B C3B -89.9(6) . . . . ? C16B S1B C2B C1B 92.3(7) . . . . ? C1B C2B C3B C4B -2.5(6) . . . . ? S1B C2B C3B C4B 179.7(6) . . . . ? C2B C3B C4B C5B 4.8(7) . . . . ? C2B C3B C4B C7B -179.1(4) . . . . ? C3B C4B C5B C6B -4.3(7) . . . . ? C7B C4B C5B C6B 179.4(5) . . . . ? C4B C5B C6B C1B 1.6(7) . . . . ? C4B C5B C6B S2B 174.5(6) . . . 2 ? C2B C1B C6B C5B 0.9(6) . . . . ? O1B C1B C6B C5B 179.9(4) . . . . ? C2B C1B C6B S2B -173.1(5) . . . 2 ? O1B C1B C6B S2B 5.9(6) . . . 2 ? C3B C4B C7B C9B 136.7(6) . . . . ? C5B C4B C7B C9B -47.4(7) . . . . ? C3B C4B C7B C8B -0.9(8) . . . . ? C5B C4B C7B C8B 175.0(5) . . . . ? C3B C4B C7B C10B -115.6(6) . . . . ? C5B C4B C7B C10B 60.3(6) . . . . ? N1A C11A C12A C13A 178.9(3) . . . . ? C16A C11A C12A C13A -3.0(4) . . . . ? N1A C11A C12A S2A 2.4(6) . . . . ? C16A C11A C12A S2A -179.6(7) . . . . ? C6A S2A C12A C11A 95.6(7) . . . . ? C6A S2A C12A C13A -80.9(7) . . . . ? C11A C12A C13A C14A 1.2(6) . . . . ? S2A C12A C13A C14A 177.6(7) . . . . ? C12A C13A C14A C15A -1.1(7) . . . . ? C12A C13A C14A C17A 178.3(4) . . . . ? C13A C14A C15A C16A 2.9(7) . . . . ? C17A C14A C15A C16A -176.5(5) . . . . ? N1A C11A C16A C15A -177.2(3) . . . . ? C12A C11A C16A C15A 4.8(5) . . . . ? N1A C11A C16A S1A -1.0(8) . . . 2 ? C12A C11A C16A S1A -179.1(7) . . . 2 ? C14A C15A C16A C11A -5.0(8) . . . . ? C14A C15A C16A S1A 178.0(6) . . . 2 ? C13A C14A C17A C18A 22.8(8) . . . . ? C15A C14A C17A C18A -157.9(6) . . . . ? C13A C14A C17A C20A -93.0(6) . . . . ? C15A C14A C17A C20A 86.4(7) . . . . ? C13A C14A C17A C19A 146.2(6) . . . . ? C15A C14A C17A C19A -34.4(7) . . . . ? N1B C11B C12B C13B 179.3(3) . . . . ? C16B C11B C12B C13B -3.9(4) . . . . ? N1B C11B C12B S2B 5.4(6) . . . . ? C16B C11B C12B S2B -177.8(6) . . . . ? C6B S2B C12B C11B 102.5(5) 2 . . . ? C6B S2B C12B C13B -71.7(5) 2 . . . ? C11B C12B C13B C14B -0.9(6) . . . . ? S2B C12B C13B C14B 173.0(6) . . . . ? C12B C13B C14B C15B 4.3(7) . . . . ? C12B C13B C14B C17B 179.5(4) . . . . ? C13B C14B C15B C16B -2.7(7) . . . . ? C17B C14B C15B C16B -177.9(4) . . . . ? N1B C11B C16B C15B -177.3(4) . . . . ? C12B C11B C16B C15B 5.5(5) . . . . ? N1B C11B C16B S1B 7.3(6) . . . . ? C12B C11B C16B S1B -169.9(5) . . . . ? C14B C15B C16B C11B -2.4(7) . . . . ? C14B C15B C16B S1B 172.4(6) . . . . ? C2B S1B C16B C11B -104.4(6) . . . . ? C2B S1B C16B C15B 80.4(8) . . . . ? C15B C14B C17B C20B -30.0(7) . . . . ? C13B C14B C17B C20B 154.9(6) . . . . ? C15B C14B C17B C18B -137.0(6) . . . . ? C13B C14B C17B C18B 47.9(7) . . . . ? C15B C14B C17B C19B 104.0(6) . . . . ? C13B C14B C17B C19B -71.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.632 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.071 _database_code_depnum_ccdc_archive 'CCDC 974895' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5c_free # start Validation Reply Form _vrf_PLAT340_12diam ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0102 Ang. RESPONSE: Two aromatic rings are completely disordered (ratio 70:30). The minor part of the disordered molecules could not be refined with perfect quality, even when using suitable restraints for the bond lengths. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H50 N2 O2 S4' _chemical_formula_sum 'C40 H50 N2 O2 S4' _chemical_formula_weight 719.06 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.019(5) _cell_length_b 15.041(7) _cell_length_c 13.613(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.487(13) _cell_angle_gamma 90.00 _cell_volume 1994.9(17) _cell_formula_units_Z 2 _cell_measurement_temperature 113 _cell_measurement_reflns_used 7771 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.44 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.273 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7177 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 113 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 27.44 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14753 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7564 _reflns_number_gt 5684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FS-PROCESS-AUTO(Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'FS-PROCESS-AUTO(Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996) and PLATON (Spek, 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita, 2001, Kabuto et al., 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1289P)^2^+1.7203P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(10) _refine_ls_number_reflns 7564 _refine_ls_number_parameters 744 _refine_ls_number_restraints 1000 _refine_ls_R_factor_all 0.1132 _refine_ls_R_factor_gt 0.0903 _refine_ls_wR_factor_ref 0.2547 _refine_ls_wR_factor_gt 0.2370 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.1568(4) 0.4556(5) -0.0135(4) 0.0433(10) Uani 1 1 d U . . C1 C 0.2812(5) 0.4555(6) -0.0389(3) 0.0353(9) Uani 1 1 d U A . C2 C 0.3490(6) 0.5359(5) -0.0470(4) 0.0367(11) Uani 1 1 d U . . C3 C 0.4758(6) 0.5369(5) -0.0742(4) 0.0391(12) Uani 1 1 d U A . H3 H 0.5197 0.5921 -0.0794 0.047 Uiso 1 1 calc R . . C4 C 0.5389(5) 0.4570(6) -0.0938(4) 0.0406(10) Uani 1 1 d U . . C5 C 0.4724(6) 0.3787(5) -0.0822(5) 0.0397(12) Uani 1 1 d U A . H5 H 0.5139 0.3240 -0.0933 0.048 Uiso 1 1 calc R . . C6 C 0.3475(6) 0.3769(5) -0.0552(4) 0.0375(11) Uani 1 1 d U . . O1 O 0.0454(4) 0.4496(5) 0.2053(3) 0.0522(10) Uani 1 1 d U . . C7 C 0.0560(5) 0.4475(6) 0.3076(3) 0.0321(9) Uani 1 1 d U K . C8 C 0.0742(6) 0.3679(5) 0.3646(4) 0.0336(11) Uani 1 1 d U . . C9 C 0.0722(6) 0.3703(5) 0.4678(4) 0.0370(11) Uani 1 1 d U K . H9 H 0.0808 0.3162 0.5047 0.044 Uiso 1 1 calc R . . C10 C 0.0582(5) 0.4485(6) 0.5165(4) 0.0361(9) Uani 1 1 d U . . C11 C 0.0531(5) 0.5267(5) 0.4613(4) 0.0317(10) Uani 1 1 d U K . H11 H 0.0508 0.5819 0.4948 0.038 Uiso 1 1 calc R . . C12 C 0.0513(5) 0.5268(5) 0.3593(4) 0.0324(11) Uani 1 1 d U . . C13A C 0.6703(11) 0.4674(9) -0.1300(8) 0.0488(17) Uani 0.61 1 d PDU A 1 C14A C 0.7730(12) 0.5204(9) -0.0502(10) 0.060(3) Uani 0.61 1 d PDU A 1 H14A H 0.7352 0.5794 -0.0427 0.090 Uiso 0.61 1 calc PR A 1 H14B H 0.8594 0.5266 -0.0716 0.090 Uiso 0.61 1 calc PR A 1 H14C H 0.7899 0.4890 0.0146 0.090 Uiso 0.61 1 calc PR A 1 C15A C 0.6445(13) 0.5188(9) -0.2317(9) 0.062(3) Uani 0.61 1 d PDU A 1 H15A H 0.6095 0.5783 -0.2227 0.093 Uiso 0.61 1 calc P B 1 H15B H 0.5771 0.4866 -0.2831 0.093 Uiso 0.61 1 calc P C 1 H15C H 0.7308 0.5239 -0.2535 0.093 Uiso 0.61 1 calc P D 1 C16A C 0.7320(11) 0.3770(8) -0.1400(10) 0.055(2) Uani 0.61 1 d PDU A 1 H16A H 0.8236 0.3845 -0.1528 0.083 Uiso 0.61 1 calc P E 1 H16B H 0.6732 0.3447 -0.1964 0.083 Uiso 0.61 1 calc P F 1 H16C H 0.7390 0.3434 -0.0774 0.083 Uiso 0.61 1 calc P G 1 C13B C 0.6869(16) 0.4470(13) -0.1149(11) 0.0504(19) Uani 0.39 1 d PDU A 2 C14B C 0.7866(17) 0.3920(13) -0.0344(14) 0.064(3) Uani 0.39 1 d PDU A 2 H14D H 0.7489 0.3322 -0.0311 0.096 Uiso 0.39 1 calc P H 2 H14E H 0.7988 0.4210 0.0315 0.096 Uiso 0.39 1 calc P I 2 H14F H 0.8755 0.3877 -0.0525 0.096 Uiso 0.39 1 calc P J 2 C15B C 0.6664(19) 0.3948(13) -0.2164(14) 0.061(3) Uani 0.39 1 d PDU A 2 H15D H 0.6193 0.4328 -0.2722 0.091 Uiso 0.39 1 calc PR A 2 H15E H 0.6110 0.3416 -0.2134 0.091 Uiso 0.39 1 calc PR A 2 H15F H 0.7561 0.3772 -0.2272 0.091 Uiso 0.39 1 calc PR A 2 C16B C 0.7516(19) 0.5368(10) -0.1227(16) 0.058(3) Uani 0.39 1 d PDU A 2 H16D H 0.8493 0.5290 -0.1205 0.087 Uiso 0.39 1 calc PR A 2 H16E H 0.7412 0.5743 -0.0660 0.087 Uiso 0.39 1 calc PR A 2 H16F H 0.7060 0.5652 -0.1864 0.087 Uiso 0.39 1 calc PR A 2 C17A C 0.0813(14) 0.4547(12) 0.6301(10) 0.0485(19) Uani 0.46 1 d PDU K 1 C18A C 0.0123(17) 0.5284(11) 0.6657(11) 0.052(3) Uani 0.46 1 d PDU K 1 H18A H 0.0726 0.5806 0.6758 0.079 Uiso 0.46 1 calc P L 1 H18B H -0.0098 0.5123 0.7299 0.079 Uiso 0.46 1 calc P M 1 H18C H -0.0725 0.5422 0.6156 0.079 Uiso 0.46 1 calc P N 1 C19A C 0.009(2) 0.3656(13) 0.6671(15) 0.058(3) Uani 0.46 1 d PDU K 1 H19A H -0.0324 0.3815 0.7230 0.087 Uiso 0.46 1 calc P O 1 H19B H 0.0795 0.3198 0.6896 0.087 Uiso 0.46 1 calc P P 1 H19C H -0.0614 0.3427 0.6105 0.087 Uiso 0.46 1 calc P Q 1 C20A C 0.2310(15) 0.4438(16) 0.6823(12) 0.078(3) Uani 0.46 1 d PDU K 1 H20A H 0.2882 0.4642 0.6373 0.117 Uiso 0.46 1 calc P R 1 H20B H 0.2502 0.3809 0.6988 0.117 Uiso 0.46 1 calc P S 1 H20C H 0.2517 0.4791 0.7445 0.117 Uiso 0.46 1 calc P T 1 C17B C 0.0412(12) 0.4527(11) 0.6269(8) 0.0468(17) Uani 0.54 1 d PDU K 2 C18B C -0.0730(15) 0.5069(10) 0.6406(10) 0.060(3) Uani 0.54 1 d PDU K 2 H18D H -0.1595 0.4761 0.6121 0.090 Uiso 0.54 1 calc P U 2 H18E H -0.0718 0.5640 0.6061 0.090 Uiso 0.54 1 calc P V 2 H18F H -0.0646 0.5173 0.7129 0.090 Uiso 0.54 1 calc P W 2 C19B C 0.1761(15) 0.5123(11) 0.6873(10) 0.069(3) Uani 0.54 1 d PDU K 2 H19D H 0.1718 0.5718 0.6574 0.104 Uiso 0.54 1 calc P X 2 H19E H 0.2610 0.4828 0.6811 0.104 Uiso 0.54 1 calc P Y 2 H19F H 0.1748 0.5173 0.7588 0.104 Uiso 0.54 1 calc P Z 2 C20B C 0.0677(17) 0.3657(10) 0.6825(12) 0.059(3) Uani 0.54 1 d PDU K 2 H20D H 0.0662 0.3748 0.7535 0.089 Uiso 0.54 1 calc PR K 2 H20E H 0.1577 0.3428 0.6782 0.089 Uiso 0.54 1 calc PR K 2 H20F H -0.0036 0.3228 0.6519 0.089 Uiso 0.54 1 calc PR K 2 O2A O 0.0460(8) 0.6178(4) 0.0743(7) 0.0392(19) Uani 0.70 1 d PDU K 1 C21A C 0.1735(8) 0.6297(3) 0.1429(6) 0.0315(12) Uani 0.70 1 d PDU K 1 C22A C 0.1785(7) 0.6341(5) 0.2448(7) 0.0349(12) Uani 0.70 1 d PDU K 1 C23A C 0.3087(8) 0.6459(5) 0.3138(6) 0.0354(14) Uani 0.70 1 d PDU K 1 H23A H 0.3125 0.6493 0.3841 0.043 Uiso 0.70 1 calc PR K 1 C24A C 0.4289(8) 0.6525(5) 0.2816(6) 0.0374(13) Uani 0.70 1 d PDU K 1 C25A C 0.4190(8) 0.6482(6) 0.1767(6) 0.0346(13) Uani 0.70 1 d PDU K 1 H25A H 0.5001 0.6531 0.1522 0.042 Uiso 0.70 1 calc PR K 1 C26A C 0.2923(9) 0.6368(7) 0.1076(6) 0.0317(11) Uani 0.70 1 d PDU K 1 C27A C 0.5672(9) 0.6672(6) 0.3574(7) 0.0501(15) Uani 0.70 1 d PDU K 1 C28A C 0.5672(12) 0.7688(9) 0.3804(9) 0.072(3) Uani 0.70 1 d PDU K 1 H28A H 0.4798 0.7853 0.3959 0.109 Uiso 0.70 1 calc P A 1 H28B H 0.5792 0.8023 0.3213 0.109 Uiso 0.70 1 calc P B 1 H28C H 0.6427 0.7826 0.4384 0.109 Uiso 0.70 1 calc P C 1 C29A C 0.6875(11) 0.6461(10) 0.3103(9) 0.069(2) Uani 0.70 1 d PDU K 1 H29A H 0.7734 0.6494 0.3623 0.104 Uiso 0.70 1 calc P D 1 H29B H 0.6900 0.6893 0.2569 0.104 Uiso 0.70 1 calc P E 1 H29C H 0.6765 0.5861 0.2815 0.104 Uiso 0.70 1 calc P F 1 C30A C 0.5812(12) 0.6196(10) 0.4548(8) 0.066(3) Uani 0.70 1 d PDU K 1 H30A H 0.5066 0.5763 0.4487 0.099 Uiso 0.70 1 calc P G 1 H30B H 0.5765 0.6625 0.5081 0.099 Uiso 0.70 1 calc P H 1 H30C H 0.6696 0.5887 0.4720 0.099 Uiso 0.70 1 calc P I 1 O2B O 0.0475(17) 0.6459(14) 0.0899(15) 0.036(3) Uani 0.30 1 d PDU K 2 C21B C 0.1817(16) 0.6448(16) 0.1507(13) 0.0321(15) Uani 0.30 1 d PDU K 2 C22B C 0.2027(15) 0.6372(18) 0.2542(13) 0.0335(15) Uani 0.30 1 d PDU K 2 C23B C 0.3389(15) 0.6208(16) 0.3118(12) 0.0367(16) Uani 0.30 1 d PDU K 2 H23B H 0.3527 0.6105 0.3823 0.044 Uiso 0.30 1 calc PR K 2 C24B C 0.4506(13) 0.6192(15) 0.2699(11) 0.0410(16) Uani 0.30 1 d PDU K 2 C25B C 0.4252(17) 0.6271(17) 0.1637(11) 0.0355(16) Uani 0.30 1 d PDU K 2 H25B H 0.4997 0.6242 0.1316 0.043 Uiso 0.30 1 calc PR K 2 C26B C 0.2916(17) 0.639(2) 0.1049(12) 0.0323(15) Uani 0.30 1 d PDU K 2 C27B C 0.5965(15) 0.6019(12) 0.3331(12) 0.054(2) Uani 0.30 1 d PDU K 2 C28B C 0.662(2) 0.6966(15) 0.3417(19) 0.069(3) Uani 0.30 1 d PDU K 2 H28D H 0.5903 0.7414 0.3397 0.104 Uiso 0.30 1 calc P J 2 H28E H 0.7055 0.7064 0.2852 0.104 Uiso 0.30 1 calc P K 2 H28F H 0.7310 0.7016 0.4056 0.104 Uiso 0.30 1 calc P L 2 C29B C 0.675(2) 0.5382(18) 0.2812(17) 0.072(4) Uani 0.30 1 d PDU K 2 H29D H 0.7661 0.5270 0.3253 0.108 Uiso 0.30 1 calc P M 2 H29E H 0.6862 0.5645 0.2177 0.108 Uiso 0.30 1 calc P N 2 H29F H 0.6250 0.4821 0.2672 0.108 Uiso 0.30 1 calc P O 2 C30B C 0.604(2) 0.5704(19) 0.4378(13) 0.060(4) Uani 0.30 1 d PDU K 2 H30D H 0.5636 0.5108 0.4355 0.091 Uiso 0.30 1 calc P P 2 H30E H 0.5525 0.6113 0.4714 0.091 Uiso 0.30 1 calc P Q 2 H30F H 0.6998 0.5683 0.4755 0.091 Uiso 0.30 1 calc P R 2 N2A N 0.0582(10) 0.2552(6) 0.0870(9) 0.047(2) Uani 0.70 1 d PDU A 1 C31A C 0.1885(9) 0.2671(4) 0.1407(7) 0.0389(12) Uani 0.70 1 d PDU A 1 C32A C 0.2258(8) 0.2737(6) 0.2499(7) 0.0397(13) Uani 0.70 1 d PDU A 1 C33A C 0.3606(9) 0.2859(6) 0.3020(7) 0.0437(14) Uani 0.70 1 d PDU A 1 H33A H 0.3819 0.2899 0.3736 0.052 Uiso 0.70 1 calc PR A 1 C34A C 0.4622(9) 0.2922(5) 0.2525(7) 0.0500(14) Uani 0.70 1 d PDU A 1 C35A C 0.4317(9) 0.2856(6) 0.1479(7) 0.0448(14) Uani 0.70 1 d PDU A 1 H35A H 0.5038 0.2898 0.1136 0.054 Uiso 0.70 1 calc PR A 1 C36A C 0.2964(10) 0.2730(7) 0.0916(7) 0.0423(13) Uani 0.70 1 d PDU A 1 C37A C 0.6184(12) 0.3067(7) 0.3138(8) 0.0675(19) Uani 0.70 1 d PDU A 1 C38A C 0.6206(15) 0.3577(11) 0.4073(11) 0.100(4) Uani 0.70 1 d PDU A 1 H38A H 0.6663 0.3225 0.4662 0.150 Uiso 0.70 1 calc P S 1 H38B H 0.5262 0.3707 0.4116 0.150 Uiso 0.70 1 calc P T 1 H38C H 0.6706 0.4135 0.4061 0.150 Uiso 0.70 1 calc P U 1 C39A C 0.6959(14) 0.2246(10) 0.3280(12) 0.088(3) Uani 0.70 1 d PDU A 1 H39A H 0.7865 0.2348 0.3143 0.132 Uiso 0.70 1 calc P V 1 H39B H 0.6468 0.1794 0.2815 0.132 Uiso 0.70 1 calc P W 1 H39C H 0.7069 0.2041 0.3977 0.132 Uiso 0.70 1 calc P X 1 C40A C 0.6851(14) 0.3657(11) 0.2436(12) 0.096(3) Uani 0.70 1 d PDU A 1 H40A H 0.7852 0.3619 0.2656 0.144 Uiso 0.70 1 calc P Y 1 H40B H 0.6562 0.4276 0.2475 0.144 Uiso 0.70 1 calc P Z 1 H40C H 0.6555 0.3447 0.1738 0.144 Uiso 0.70 1 calc P A 1 N2B N 0.0488(17) 0.2838(9) 0.0755(15) 0.031(3) Uani 0.30 1 d PDU A 2 C31B C 0.1755(17) 0.2749(6) 0.1367(14) 0.0401(15) Uani 0.30 1 d PDU A 2 C32B C 0.1978(16) 0.2685(11) 0.2454(14) 0.0398(15) Uani 0.30 1 d PDU A 2 C33B C 0.3271(16) 0.2595(11) 0.3076(13) 0.0425(18) Uani 0.30 1 d PDU A 2 H33B H 0.3378 0.2552 0.3787 0.051 Uiso 0.30 1 calc PR A 2 C34B C 0.4381(15) 0.2567(9) 0.2680(12) 0.0487(16) Uani 0.30 1 d PDU A 2 C35B C 0.4232(18) 0.2619(12) 0.1638(12) 0.0453(17) Uani 0.30 1 d PDU A 2 H35B H 0.5024 0.2593 0.1368 0.054 Uiso 0.30 1 calc PR A 2 C36B C 0.2930(19) 0.2709(12) 0.0978(13) 0.0422(16) Uani 0.30 1 d PDU A 2 C37B C 0.5894(17) 0.2451(12) 0.3397(14) 0.064(2) Uani 0.30 1 d PDU A 2 C38B C 0.607(3) 0.2928(19) 0.4369(18) 0.085(5) Uani 0.30 1 d PDU A 2 H38D H 0.5635 0.3514 0.4250 0.128 Uiso 0.30 1 calc P B 2 H38E H 0.7049 0.2999 0.4677 0.128 Uiso 0.30 1 calc P C 2 H38F H 0.5637 0.2585 0.4824 0.128 Uiso 0.30 1 calc P D 2 C39B C 0.691(2) 0.262(2) 0.281(2) 0.084(3) Uani 0.30 1 d PDU A 2 H39D H 0.7146 0.2063 0.2525 0.127 Uiso 0.30 1 calc P E 2 H39E H 0.7734 0.2878 0.3254 0.127 Uiso 0.30 1 calc P F 2 H39F H 0.6531 0.3040 0.2267 0.127 Uiso 0.30 1 calc P G 2 C40B C 0.599(3) 0.1433(15) 0.365(2) 0.079(5) Uani 0.30 1 d PDU A 2 H40D H 0.5140 0.1138 0.3297 0.119 Uiso 0.30 1 calc P H 2 H40E H 0.6113 0.1352 0.4381 0.119 Uiso 0.30 1 calc P I 2 H40F H 0.6769 0.1174 0.3434 0.119 Uiso 0.30 1 calc P J 2 S1A S 0.2768(15) 0.6440(8) -0.0217(8) 0.0397(16) Uani 0.70 1 d PU K 1 S2A S 0.0271(3) 0.6280(4) 0.2909(3) 0.0390(9) Uani 0.70 1 d PU K 1 S3A S 0.0874(3) 0.2606(3) 0.3127(3) 0.0385(7) Uani 0.70 1 d PU A 1 S4A S 0.2777(11) 0.2694(9) -0.0409(12) 0.0430(18) Uani 0.70 1 d PU A 1 S1B S 0.271(3) 0.630(2) -0.039(2) 0.037(3) Uani 0.30 1 d PU K 2 S2B S 0.0691(9) 0.6377(10) 0.3120(9) 0.0357(16) Uani 0.30 1 d PU K 2 S3B S 0.0303(9) 0.2709(7) 0.2833(7) 0.0498(17) Uani 0.30 1 d PU A 2 S4B S 0.252(3) 0.2813(19) -0.042(3) 0.037(3) Uani 0.30 1 d PU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.033(2) 0.048(3) 0.053(3) 0.003(3) 0.0201(18) -0.006(3) C1 0.032(2) 0.046(2) 0.0286(19) -0.004(2) 0.0094(16) -0.004(2) C2 0.040(2) 0.042(3) 0.029(2) 0.004(2) 0.0095(19) -0.002(2) C3 0.037(2) 0.043(3) 0.038(2) 0.003(2) 0.0112(19) -0.006(2) C4 0.033(2) 0.048(2) 0.043(2) 0.000(2) 0.0128(17) -0.002(2) C5 0.039(2) 0.043(3) 0.041(2) -0.006(2) 0.016(2) 0.001(2) C6 0.037(2) 0.046(3) 0.033(2) -0.007(2) 0.0140(19) -0.009(2) O1 0.060(2) 0.066(3) 0.0337(19) 0.002(3) 0.0174(17) -0.008(3) C7 0.0280(19) 0.039(2) 0.0318(19) 0.000(2) 0.0132(15) 0.003(2) C8 0.033(2) 0.035(3) 0.038(2) 0.000(2) 0.0187(18) 0.002(2) C9 0.038(2) 0.036(3) 0.039(2) 0.003(2) 0.0141(19) 0.001(2) C10 0.036(2) 0.042(2) 0.0312(18) -0.003(2) 0.0095(15) 0.003(2) C11 0.028(2) 0.034(3) 0.033(2) -0.007(2) 0.0076(17) -0.001(2) C12 0.022(2) 0.037(3) 0.040(2) 0.004(2) 0.0112(17) 0.003(2) C13A 0.036(3) 0.054(4) 0.061(3) -0.001(3) 0.020(3) -0.002(3) C14A 0.044(5) 0.058(5) 0.071(5) -0.003(5) 0.000(4) -0.007(4) C15A 0.053(5) 0.072(6) 0.070(6) 0.008(5) 0.033(4) -0.002(5) C16A 0.039(4) 0.052(5) 0.082(5) -0.005(5) 0.030(4) 0.004(4) C13B 0.036(3) 0.055(4) 0.063(3) -0.001(3) 0.018(3) -0.001(3) C14B 0.034(6) 0.064(7) 0.092(7) 0.008(7) 0.013(6) 0.003(6) C15B 0.047(5) 0.064(6) 0.080(6) -0.005(6) 0.033(5) -0.004(5) C16B 0.043(5) 0.061(5) 0.070(5) -0.002(5) 0.013(5) -0.002(5) C17A 0.054(4) 0.058(3) 0.035(3) -0.007(3) 0.012(3) 0.001(4) C18A 0.062(5) 0.062(5) 0.037(4) -0.014(4) 0.020(4) -0.007(5) C19A 0.070(7) 0.064(6) 0.041(5) -0.002(5) 0.016(5) 0.000(6) C20A 0.075(7) 0.096(7) 0.052(6) -0.009(7) -0.007(5) 0.002(7) C17B 0.051(4) 0.057(3) 0.034(3) -0.008(3) 0.013(3) 0.001(3) C18B 0.068(6) 0.071(6) 0.045(5) -0.013(5) 0.019(5) -0.001(6) C19B 0.076(5) 0.076(5) 0.046(5) -0.010(5) -0.006(4) -0.012(5) C20B 0.070(6) 0.063(5) 0.042(5) -0.005(4) 0.009(5) -0.003(6) O2A 0.036(3) 0.039(5) 0.040(4) 0.008(3) 0.005(2) 0.009(3) C21A 0.031(2) 0.027(3) 0.037(2) 0.007(2) 0.0086(19) 0.005(2) C22A 0.033(2) 0.030(2) 0.042(2) 0.004(2) 0.009(2) 0.005(2) C23A 0.033(3) 0.033(3) 0.040(2) 0.001(2) 0.008(2) 0.003(2) C24A 0.036(2) 0.037(3) 0.040(2) -0.001(2) 0.009(2) 0.003(2) C25A 0.034(2) 0.033(3) 0.039(2) 0.004(2) 0.0138(19) 0.002(2) C26A 0.035(2) 0.029(2) 0.033(2) 0.008(2) 0.0110(19) 0.005(2) C27A 0.041(3) 0.055(3) 0.051(3) 0.001(3) 0.005(2) 0.000(3) C28A 0.060(5) 0.084(6) 0.062(5) -0.017(5) -0.009(4) -0.011(5) C29A 0.049(4) 0.079(5) 0.071(5) -0.006(5) -0.004(4) -0.006(4) C30A 0.061(5) 0.077(6) 0.055(5) -0.004(5) 0.003(4) -0.004(5) O2B 0.035(5) 0.035(6) 0.034(5) 0.011(5) 0.003(4) 0.006(5) C21B 0.032(2) 0.028(3) 0.037(3) 0.007(2) 0.008(2) 0.005(3) C22B 0.032(3) 0.030(3) 0.039(3) 0.005(3) 0.010(2) 0.004(3) C23B 0.034(3) 0.034(3) 0.041(3) 0.003(3) 0.006(3) 0.003(3) C24B 0.036(3) 0.042(3) 0.044(3) 0.003(3) 0.007(2) 0.000(3) C25B 0.035(3) 0.034(3) 0.039(3) 0.004(3) 0.010(2) 0.002(3) C26B 0.034(3) 0.029(3) 0.035(3) 0.007(3) 0.011(2) 0.004(3) C27B 0.044(4) 0.059(4) 0.055(4) 0.003(4) 0.000(3) -0.003(4) C28B 0.054(5) 0.074(6) 0.069(6) -0.008(5) -0.010(5) -0.010(5) C29B 0.054(7) 0.079(8) 0.074(7) 0.005(7) -0.004(7) -0.001(7) C30B 0.056(7) 0.066(8) 0.053(7) 0.000(7) -0.001(6) 0.000(7) N2A 0.044(3) 0.039(5) 0.062(4) -0.008(4) 0.016(3) -0.011(4) C31A 0.046(2) 0.024(2) 0.053(2) -0.014(2) 0.024(2) -0.007(2) C32A 0.045(3) 0.027(2) 0.054(2) -0.013(2) 0.025(2) -0.006(2) C33A 0.047(3) 0.032(3) 0.055(3) -0.012(2) 0.018(2) -0.007(2) C34A 0.051(3) 0.043(3) 0.059(3) -0.008(2) 0.017(2) -0.007(2) C35A 0.048(3) 0.036(3) 0.056(3) -0.011(2) 0.024(2) -0.004(2) C36A 0.048(2) 0.031(3) 0.054(3) -0.015(2) 0.024(2) -0.005(2) C37A 0.060(3) 0.068(4) 0.072(4) -0.006(3) 0.011(3) -0.009(3) C38A 0.080(6) 0.110(8) 0.100(7) -0.038(6) 0.002(6) -0.023(6) C39A 0.074(5) 0.085(6) 0.097(6) 0.018(5) 0.005(5) 0.001(5) C40A 0.074(6) 0.100(7) 0.102(7) 0.013(6) -0.005(5) -0.024(6) N2B 0.038(5) 0.018(6) 0.048(5) -0.011(5) 0.031(4) -0.006(5) C31B 0.046(3) 0.027(3) 0.054(3) -0.013(2) 0.025(2) -0.007(3) C32B 0.046(3) 0.027(3) 0.052(3) -0.012(2) 0.024(2) -0.008(2) C33B 0.047(3) 0.032(3) 0.054(3) -0.011(3) 0.023(3) -0.006(3) C34B 0.051(3) 0.040(3) 0.058(3) -0.011(3) 0.020(3) -0.005(3) C35B 0.049(3) 0.036(3) 0.056(3) -0.011(3) 0.022(3) -0.005(3) C36B 0.048(3) 0.031(3) 0.054(3) -0.013(3) 0.024(3) -0.006(3) C37B 0.061(3) 0.060(4) 0.071(4) -0.008(3) 0.013(3) -0.003(3) C38B 0.076(8) 0.084(8) 0.087(8) -0.028(8) -0.001(7) -0.013(8) C39B 0.071(6) 0.084(6) 0.091(6) 0.005(6) 0.004(6) -0.006(6) C40B 0.078(9) 0.075(10) 0.077(9) -0.003(9) 0.005(9) 0.011(9) S1A 0.0601(16) 0.031(3) 0.033(4) 0.006(2) 0.020(3) 0.008(2) S2A 0.031(2) 0.0401(19) 0.051(2) 0.0130(16) 0.0206(15) 0.0116(18) S3A 0.0468(16) 0.0281(13) 0.0447(16) -0.0065(11) 0.0191(12) -0.0106(14) S4A 0.044(4) 0.042(4) 0.0496(14) -0.021(2) 0.026(3) -0.008(2) S1B 0.059(4) 0.034(6) 0.028(6) 0.004(4) 0.028(4) 0.011(4) S2B 0.029(4) 0.031(3) 0.050(3) 0.008(3) 0.014(3) 0.008(3) S3B 0.069(4) 0.033(3) 0.061(4) -0.013(3) 0.041(3) -0.024(4) S4B 0.043(6) 0.031(5) 0.048(3) -0.025(4) 0.032(5) -0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.369(6) . ? C1 C6 1.398(10) . ? C1 C2 1.405(10) . ? C2 C3 1.403(8) . ? C2 S1B 1.64(3) . ? C2 S1A 1.845(13) . ? C3 C4 1.413(10) . ? C3 H3 0.9500 . ? C4 C5 1.380(10) . ? C4 C13A 1.517(12) . ? C4 C13B 1.582(16) . ? C5 C6 1.386(8) . ? C5 H5 0.9500 . ? C6 S4B 1.76(3) . ? C6 S4A 1.790(16) . ? O1 C7 1.372(6) . ? C7 C12 1.392(9) . ? C7 C8 1.414(9) . ? C8 C9 1.410(8) . ? C8 S3A 1.780(7) . ? C8 S3B 1.822(11) . ? C9 C10 1.374(9) . ? C9 H9 0.9500 . ? C10 C11 1.389(9) . ? C10 C17A 1.513(14) . ? C10 C17B 1.554(12) . ? C11 C12 1.384(8) . ? C11 H11 0.9500 . ? C12 S2A 1.772(8) . ? C12 S2B 1.812(15) . ? C13A C16A 1.512(16) . ? C13A C14A 1.533(13) . ? C13A C15A 1.554(14) . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C13B C16B 1.511(17) . ? C13B C14B 1.540(14) . ? C13B C15B 1.560(15) . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17A C18A 1.448(15) . ? C17A C20A 1.511(17) . ? C17A C19A 1.655(19) . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C17B C18B 1.452(14) . ? C17B C20B 1.504(17) . ? C17B C19B 1.670(18) . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? O2A C21A 1.407(7) . ? C21A C22A 1.378(8) . ? C21A C26A 1.388(8) . ? C22A C23A 1.430(9) . ? C22A S2A 1.774(9) . ? C23A C24A 1.378(10) . ? C23A H23A 0.9500 . ? C24A C25A 1.409(9) . ? C24A C27A 1.539(10) . ? C25A C26A 1.404(9) . ? C25A H25A 0.9500 . ? C26A S1A 1.734(14) . ? C27A C30A 1.484(13) . ? C27A C29A 1.525(15) . ? C27A C28A 1.560(15) . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C30A H30A 0.9800 . ? C30A H30B 0.9800 . ? C30A H30C 0.9800 . ? O2B C21B 1.404(10) . ? C21B C22B 1.380(10) . ? C21B C26B 1.389(10) . ? C22B C23B 1.429(12) . ? C22B S2B 1.704(19) . ? C23B C24B 1.370(13) . ? C23B H23B 0.9500 . ? C24B C25B 1.413(12) . ? C24B C27B 1.536(12) . ? C25B C26B 1.401(11) . ? C25B H25B 0.9500 . ? C26B S1B 1.92(3) . ? C27B C30B 1.488(15) . ? C27B C29B 1.517(17) . ? C27B C28B 1.562(17) . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? N2A C31A 1.352(9) . ? C31A C36A 1.400(9) . ? C31A C32A 1.449(9) . ? C32A C33A 1.384(11) . ? C32A S3A 1.802(9) . ? C33A C34A 1.350(12) . ? C33A H33A 0.9500 . ? C34A C35A 1.387(11) . ? C34A C37A 1.607(13) . ? C35A C36A 1.406(10) . ? C35A H35A 0.9500 . ? C36A S4A 1.770(18) . ? C37A C39A 1.447(15) . ? C37A C38A 1.482(16) . ? C37A C40A 1.563(17) . ? C38A H38A 0.9800 . ? C38A H38B 0.9800 . ? C38A H38C 0.9800 . ? C39A H39A 0.9800 . ? C39A H39B 0.9800 . ? C39A H39C 0.9800 . ? C40A H40A 0.9800 . ? C40A H40B 0.9800 . ? C40A H40C 0.9800 . ? N2B C31B 1.352(11) . ? C31B C36B 1.399(11) . ? C31B C32B 1.447(11) . ? C32B C33B 1.380(13) . ? C32B S3B 1.868(18) . ? C33B C34B 1.345(14) . ? C33B H33B 0.9500 . ? C34B C35B 1.393(13) . ? C34B C37B 1.610(15) . ? C35B C36B 1.407(12) . ? C35B H35B 0.9500 . ? C36B S4B 1.86(4) . ? C37B C39B 1.452(17) . ? C37B C38B 1.479(18) . ? C37B C40B 1.567(19) . ? C38B H38D 0.9800 . ? C38B H38E 0.9800 . ? C38B H38F 0.9800 . ? C39B H39D 0.9800 . ? C39B H39E 0.9800 . ? C39B H39F 0.9800 . ? C40B H40D 0.9800 . ? C40B H40E 0.9800 . ? C40B H40F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C6 122.4(7) . . ? N1 C1 C2 120.3(7) . . ? C6 C1 C2 117.3(4) . . ? C3 C2 C1 121.0(6) . . ? C3 C2 S1B 118.8(12) . . ? C1 C2 S1B 119.8(12) . . ? C3 C2 S1A 117.3(7) . . ? C1 C2 S1A 121.7(6) . . ? C2 C3 C4 120.9(6) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 117.1(4) . . ? C5 C4 C13A 127.1(8) . . ? C3 C4 C13A 115.8(7) . . ? C5 C4 C13B 116.0(9) . . ? C3 C4 C13B 126.5(9) . . ? C4 C5 C6 122.5(6) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 121.2(6) . . ? C5 C6 S4B 126.1(9) . . ? C1 C6 S4B 112.6(9) . . ? C5 C6 S4A 116.5(6) . . ? C1 C6 S4A 122.3(5) . . ? O1 C7 C12 119.3(6) . . ? O1 C7 C8 123.1(6) . . ? C12 C7 C8 117.6(4) . . ? C9 C8 C7 119.7(5) . . ? C9 C8 S3A 115.9(5) . . ? C7 C8 S3A 124.2(4) . . ? C9 C8 S3B 124.6(5) . . ? C7 C8 S3B 111.3(5) . . ? C10 C9 C8 121.9(6) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C11 117.3(4) . . ? C9 C10 C17A 122.5(8) . . ? C11 C10 C17A 118.6(8) . . ? C9 C10 C17B 123.2(8) . . ? C11 C10 C17B 119.4(8) . . ? C12 C11 C10 122.2(5) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C11 C12 C7 120.8(5) . . ? C11 C12 S2A 119.8(5) . . ? C7 C12 S2A 119.2(5) . . ? C11 C12 S2B 112.2(6) . . ? C7 C12 S2B 126.3(6) . . ? C16A C13A C4 109.9(9) . . ? C16A C13A C14A 108.1(9) . . ? C4 C13A C14A 108.3(9) . . ? C16A C13A C15A 110.7(9) . . ? C4 C13A C15A 111.4(8) . . ? C14A C13A C15A 108.5(10) . . ? C13A C15A H15A 109.5 . . ? C13A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C13A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C13A C16A H16A 109.5 . . ? C13A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C13A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C16B C13B C14B 108.2(12) . . ? C16B C13B C15B 111.0(12) . . ? C14B C13B C15B 106.8(13) . . ? C16B C13B C4 111.3(13) . . ? C14B C13B C4 113.7(12) . . ? C15B C13B C4 105.8(11) . . ? C13B C14B H14D 109.5 . . ? C13B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C13B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C13B C15B H15D 109.5 . . ? C13B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C13B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C13B C16B H16D 109.5 . . ? C13B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C13B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C18A C17A C20A 115.2(13) . . ? C18A C17A C10 114.7(11) . . ? C20A C17A C10 111.8(10) . . ? C18A C17A C19A 104.1(11) . . ? C20A C17A C19A 102.9(12) . . ? C10 C17A C19A 106.7(12) . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C17A C19A H19A 109.5 . . ? C17A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C17A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C17A C20A H20A 109.5 . . ? C17A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C17A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C18B C17B C20B 118.5(12) . . ? C18B C17B C10 114.5(9) . . ? C20B C17B C10 113.9(11) . . ? C18B C17B C19B 101.9(10) . . ? C20B C17B C19B 101.1(10) . . ? C10 C17B C19B 103.8(9) . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5 . . ? C17B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C17B C20B H20D 109.5 . . ? C17B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C17B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C22A C21A C26A 120.8(6) . . ? C22A C21A O2A 119.3(6) . . ? C26A C21A O2A 119.9(6) . . ? C21A C22A C23A 118.8(6) . . ? C21A C22A S2A 121.3(5) . . ? C23A C22A S2A 119.9(6) . . ? C24A C23A C22A 122.1(7) . . ? C24A C23A H23A 119.0 . . ? C22A C23A H23A 119.0 . . ? C23A C24A C25A 117.4(6) . . ? C23A C24A C27A 120.9(7) . . ? C25A C24A C27A 121.7(7) . . ? C26A C25A C24A 121.5(6) . . ? C26A C25A H25A 119.2 . . ? C24A C25A H25A 119.2 . . ? C21A C26A C25A 119.5(6) . . ? C21A C26A S1A 118.4(7) . . ? C25A C26A S1A 121.7(8) . . ? C30A C27A C29A 110.9(8) . . ? C30A C27A C24A 114.4(7) . . ? C29A C27A C24A 111.4(7) . . ? C30A C27A C28A 107.3(9) . . ? C29A C27A C28A 108.9(8) . . ? C24A C27A C28A 103.5(6) . . ? C27A C28A H28A 109.5 . . ? C27A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C27A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C27A C30A H30A 109.5 . . ? C27A C30A H30B 109.5 . . ? H30A C30A H30B 109.5 . . ? C27A C30A H30C 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C22B C21B C26B 120.3(9) . . ? C22B C21B O2B 120.0(11) . . ? C26B C21B O2B 119.1(11) . . ? C21B C22B C23B 118.3(10) . . ? C21B C22B S2B 121.5(10) . . ? C23B C22B S2B 120.0(11) . . ? C24B C23B C22B 122.8(11) . . ? C24B C23B H23B 118.6 . . ? C22B C23B H23B 118.6 . . ? C23B C24B C25B 117.1(10) . . ? C23B C24B C27B 122.2(11) . . ? C25B C24B C27B 120.6(11) . . ? C26B C25B C24B 121.0(10) . . ? C26B C25B H25B 119.5 . . ? C24B C25B H25B 119.5 . . ? C21B C26B C25B 120.2(10) . . ? C21B C26B S1B 123.7(14) . . ? C25B C26B S1B 115.6(15) . . ? C30B C27B C29B 109.3(13) . . ? C30B C27B C24B 114.7(12) . . ? C29B C27B C24B 112.2(12) . . ? C30B C27B C28B 107.0(14) . . ? C29B C27B C28B 110.9(13) . . ? C24B C27B C28B 102.4(11) . . ? C27B C28B H28D 109.5 . . ? C27B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C27B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C27B C30B H30D 109.5 . . ? C27B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C27B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? N2A C31A C36A 120.4(7) . . ? N2A C31A C32A 123.3(7) . . ? C36A C31A C32A 116.3(6) . . ? C33A C32A C31A 121.5(7) . . ? C33A C32A S3A 122.5(7) . . ? C31A C32A S3A 115.9(6) . . ? C34A C33A C32A 120.9(8) . . ? C34A C33A H33A 119.6 . . ? C32A C33A H33A 119.6 . . ? C33A C34A C35A 119.7(8) . . ? C33A C34A C37A 120.4(8) . . ? C35A C34A C37A 119.8(8) . . ? C34A C35A C36A 121.6(7) . . ? C34A C35A H35A 119.2 . . ? C36A C35A H35A 119.2 . . ? C31A C36A C35A 120.1(7) . . ? C31A C36A S4A 125.1(7) . . ? C35A C36A S4A 114.8(7) . . ? C39A C37A C38A 115.3(11) . . ? C39A C37A C40A 105.9(11) . . ? C38A C37A C40A 108.0(10) . . ? C39A C37A C34A 112.4(8) . . ? C38A C37A C34A 109.5(9) . . ? C40A C37A C34A 105.2(8) . . ? C37A C38A H38A 109.5 . . ? C37A C38A H38B 109.5 . . ? H38A C38A H38B 109.5 . . ? C37A C38A H38C 109.5 . . ? H38A C38A H38C 109.5 . . ? H38B C38A H38C 109.5 . . ? C37A C39A H39A 109.5 . . ? C37A C39A H39B 109.5 . . ? H39A C39A H39B 109.5 . . ? C37A C39A H39C 109.5 . . ? H39A C39A H39C 109.5 . . ? H39B C39A H39C 109.5 . . ? C37A C40A H40A 109.5 . . ? C37A C40A H40B 109.5 . . ? H40A C40A H40B 109.5 . . ? C37A C40A H40C 109.5 . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? N2B C31B C36B 121.6(11) . . ? N2B C31B C32B 122.3(11) . . ? C36B C31B C32B 116.1(10) . . ? C33B C32B C31B 122.3(11) . . ? C33B C32B S3B 127.4(12) . . ? C31B C32B S3B 110.3(10) . . ? C34B C33B C32B 120.1(12) . . ? C34B C33B H33B 119.9 . . ? C32B C33B H33B 119.9 . . ? C33B C34B C35B 120.3(11) . . ? C33B C34B C37B 120.7(11) . . ? C35B C34B C37B 119.1(11) . . ? C34B C35B C36B 121.3(11) . . ? C34B C35B H35B 119.4 . . ? C36B C35B H35B 119.4 . . ? C31B C36B C35B 119.9(11) . . ? C31B C36B S4B 112.3(13) . . ? C35B C36B S4B 127.7(14) . . ? C39B C37B C38B 116.9(15) . . ? C39B C37B C40B 106.3(14) . . ? C38B C37B C40B 106.7(13) . . ? C39B C37B C34B 109.3(12) . . ? C38B C37B C34B 112.8(13) . . ? C40B C37B C34B 103.8(11) . . ? C37B C38B H38D 109.5 . . ? C37B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C37B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? C37B C39B H39D 109.5 . . ? C37B C39B H39E 109.5 . . ? H39D C39B H39E 109.5 . . ? C37B C39B H39F 109.5 . . ? H39D C39B H39F 109.5 . . ? H39E C39B H39F 109.5 . . ? C37B C40B H40D 109.5 . . ? C37B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C37B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? C26A S1A C2 100.9(8) . . ? C12 S2A C22A 102.0(4) . . ? C8 S3A C32A 103.0(3) . . ? C36A S4A C6 97.6(8) . . ? C2 S1B C26B 101.0(19) . . ? C22B S2B C12 108.2(11) . . ? C8 S3B C32B 94.5(7) . . ? C6 S4B C36B 100.4(16) . . ? 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 N1 C1 C2 C3 -179.2(5) . . . . ? C6 C1 C2 C3 2.3(7) . . . . ? N1 C1 C2 S1B -6.9(13) . . . . ? C6 C1 C2 S1B 174.6(12) . . . . ? N1 C1 C2 S1A 1.3(8) . . . . ? C6 C1 C2 S1A -177.2(6) . . . . ? C1 C2 C3 C4 -0.2(9) . . . . ? S1B C2 C3 C4 -172.5(12) . . . . ? S1A C2 C3 C4 179.3(6) . . . . ? C2 C3 C4 C5 -1.8(8) . . . . ? C2 C3 C4 C13A 175.6(6) . . . . ? C2 C3 C4 C13B -173.8(8) . . . . ? C3 C4 C5 C6 1.6(8) . . . . ? C13A C4 C5 C6 -175.4(7) . . . . ? C13B C4 C5 C6 174.5(7) . . . . ? C4 C5 C6 C1 0.6(9) . . . . ? C4 C5 C6 S4B 178.2(15) . . . . ? C4 C5 C6 S4A -178.7(7) . . . . ? N1 C1 C6 C5 179.0(5) . . . . ? C2 C1 C6 C5 -2.5(7) . . . . ? N1 C1 C6 S4B 1.1(14) . . . . ? C2 C1 C6 S4B 179.6(13) . . . . ? N1 C1 C6 S4A -1.8(9) . . . . ? C2 C1 C6 S4A 176.7(7) . . . . ? O1 C7 C8 C9 -174.5(5) . . . . ? C12 C7 C8 C9 6.6(7) . . . . ? O1 C7 C8 S3A 0.6(7) . . . . ? C12 C7 C8 S3A -178.3(4) . . . . ? O1 C7 C8 S3B -17.1(7) . . . . ? C12 C7 C8 S3B 164.0(5) . . . . ? C7 C8 C9 C10 -2.5(8) . . . . ? S3A C8 C9 C10 -178.0(5) . . . . ? S3B C8 C9 C10 -156.6(6) . . . . ? C8 C9 C10 C11 -3.3(8) . . . . ? C8 C9 C10 C17A -168.7(8) . . . . ? C8 C9 C10 C17B 173.8(7) . . . . ? C9 C10 C11 C12 5.0(7) . . . . ? C17A C10 C11 C12 170.9(7) . . . . ? C17B C10 C11 C12 -172.2(6) . . . . ? C10 C11 C12 C7 -0.7(8) . . . . ? C10 C11 C12 S2A 173.6(4) . . . . ? C10 C11 C12 S2B -171.8(5) . . . . ? O1 C7 C12 C11 176.0(5) . . . . ? C8 C7 C12 C11 -5.1(7) . . . . ? O1 C7 C12 S2A 1.6(7) . . . . ? C8 C7 C12 S2A -179.4(4) . . . . ? O1 C7 C12 S2B -14.3(8) . . . . ? C8 C7 C12 S2B 164.6(5) . . . . ? C5 C4 C13A C16A -7.3(11) . . . . ? C3 C4 C13A C16A 175.6(8) . . . . ? C13B C4 C13A C16A 33(3) . . . . ? C5 C4 C13A C14A -125.1(9) . . . . ? C3 C4 C13A C14A 57.8(10) . . . . ? C13B C4 C13A C14A -85(3) . . . . ? C5 C4 C13A C15A 115.7(10) . . . . ? C3 C4 C13A C15A -61.4(11) . . . . ? C13B C4 C13A C15A 156(4) . . . . ? C5 C4 C13B C16B -178.1(9) . . . . ? C3 C4 C13B C16B -6.0(14) . . . . ? C13A C4 C13B C16B 37(3) . . . . ? C5 C4 C13B C14B -55.6(14) . . . . ? C3 C4 C13B C14B 116.5(13) . . . . ? C13A C4 C13B C14B 160(5) . . . . ? C5 C4 C13B C15B 61.3(12) . . . . ? C3 C4 C13B C15B -126.6(11) . . . . ? C13A C4 C13B C15B -84(3) . . . . ? C9 C10 C17A C18A -156.6(10) . . . . ? C11 C10 C17A C18A 38.2(15) . . . . ? C17B C10 C17A C18A -59(3) . . . . ? C9 C10 C17A C20A 69.9(15) . . . . ? C11 C10 C17A C20A -95.3(13) . . . . ? C17B C10 C17A C20A 167(5) . . . . ? C9 C10 C17A C19A -41.9(12) . . . . ? C11 C10 C17A C19A 152.9(9) . . . . ? C17B C10 C17A C19A 56(4) . . . . ? C9 C10 C17B C18B -129.9(11) . . . . ? C11 C10 C17B C18B 47.1(13) . . . . ? C17A C10 C17B C18B 138(5) . . . . ? C9 C10 C17B C20B 10.8(13) . . . . ? C11 C10 C17B C20B -172.2(9) . . . . ? C17A C10 C17B C20B -81(4) . . . . ? C9 C10 C17B C19B 119.8(9) . . . . ? C11 C10 C17B C19B -63.2(10) . . . . ? C17A C10 C17B C19B 28(4) . . . . ? C26A C21A C22A C23A -0.3(4) . . . . ? O2A C21A C22A C23A 179.8(3) . . . . ? C26A C21A C22A S2A 178.3(7) . . . . ? O2A C21A C22A S2A -1.6(7) . . . . ? C21A C22A C23A C24A -0.3(6) . . . . ? S2A C22A C23A C24A -178.9(7) . . . . ? C22A C23A C24A C25A 0.7(7) . . . . ? C22A C23A C24A C27A 178.6(4) . . . . ? C23A C24A C25A C26A -0.6(8) . . . . ? C27A C24A C25A C26A -178.5(5) . . . . ? C22A C21A C26A C25A 0.4(6) . . . . ? O2A C21A C26A C25A -179.7(4) . . . . ? C22A C21A C26A S1A -172.4(8) . . . . ? O2A C21A C26A S1A 7.6(9) . . . . ? C24A C25A C26A C21A 0.1(8) . . . . ? C24A C25A C26A S1A 172.6(8) . . . . ? C23A C24A C27A C30A 37.0(10) . . . . ? C25A C24A C27A C30A -145.1(9) . . . . ? C23A C24A C27A C29A 163.7(8) . . . . ? C25A C24A C27A C29A -18.4(9) . . . . ? C23A C24A C27A C28A -79.4(9) . . . . ? C25A C24A C27A C28A 98.5(8) . . . . ? C26B C21B C22B C23B -2(3) . . . . ? O2B C21B C22B C23B 169(2) . . . . ? C26B C21B C22B S2B -176(2) . . . . ? O2B C21B C22B S2B -5(3) . . . . ? C21B C22B C23B C24B 5(4) . . . . ? S2B C22B C23B C24B 180(2) . . . . ? C22B C23B C24B C25B -5(3) . . . . ? C22B C23B C24B C27B 180(2) . . . . ? C23B C24B C25B C26B 2(3) . . . . ? C27B C24B C25B C26B 177(2) . . . . ? C22B C21B C26B C25B -1(4) . . . . ? O2B C21B C26B C25B -172(2) . . . . ? C22B C21B C26B S1B 170(2) . . . . ? O2B C21B C26B S1B -1(4) . . . . ? C24B C25B C26B C21B 1(4) . . . . ? C24B C25B C26B S1B -171(2) . . . . ? C23B C24B C27B C30B 11(3) . . . . ? C25B C24B C27B C30B -164(2) . . . . ? C23B C24B C27B C29B 137(2) . . . . ? C25B C24B C27B C29B -38(2) . . . . ? C23B C24B C27B C28B -105(2) . . . . ? C25B C24B C27B C28B 81(2) . . . . ? N2A C31A C32A C33A -179.9(3) . . . . ? C36A C31A C32A C33A 0.5(4) . . . . ? N2A C31A C32A S3A 2.5(6) . . . . ? C36A C31A C32A S3A -177.1(6) . . . . ? C31A C32A C33A C34A 0.1(6) . . . . ? S3A C32A C33A C34A 177.6(6) . . . . ? C32A C33A C34A C35A -0.6(8) . . . . ? C32A C33A C34A C37A 179.8(4) . . . . ? C33A C34A C35A C36A 0.4(8) . . . . ? C37A C34A C35A C36A -180.0(5) . . . . ? N2A C31A C36A C35A 179.8(4) . . . . ? C32A C31A C36A C35A -0.6(6) . . . . ? N2A C31A C36A S4A 1.9(9) . . . . ? C32A C31A C36A S4A -178.5(8) . . . . ? C34A C35A C36A C31A 0.2(8) . . . . ? C34A C35A C36A S4A 178.3(8) . . . . ? C33A C34A C37A C39A 98.9(11) . . . . ? C35A C34A C37A C39A -80.7(11) . . . . ? C33A C34A C37A C38A -30.5(11) . . . . ? C35A C34A C37A C38A 149.9(9) . . . . ? C33A C34A C37A C40A -146.3(9) . . . . ? C35A C34A C37A C40A 34.1(10) . . . . ? N2B C31B C32B C33B -179.9(3) . . . . ? C36B C31B C32B C33B 0.3(4) . . . . ? N2B C31B C32B S3B 1.8(12) . . . . ? C36B C31B C32B S3B -178.0(12) . . . . ? C31B C32B C33B C34B 0.3(7) . . . . ? S3B C32B C33B C34B 178.3(14) . . . . ? C32B C33B C34B C35B -0.7(9) . . . . ? C32B C33B C34B C37B -179.4(5) . . . . ? C33B C34B C35B C36B 0.5(9) . . . . ? C37B C34B C35B C36B 179.2(5) . . . . ? N2B C31B C36B C35B 179.7(4) . . . . ? C32B C31B C36B C35B -0.5(6) . . . . ? N2B C31B C36B S4B 1.0(16) . . . . ? C32B C31B C36B S4B -179.2(15) . . . . ? C34B C35B C36B C31B 0.1(9) . . . . ? C34B C35B C36B S4B 178.6(18) . . . . ? C33B C34B C37B C39B -168.5(15) . . . . ? C35B C34B C37B C39B 12.9(16) . . . . ? C33B C34B C37B C38B -36.7(16) . . . . ? C35B C34B C37B C38B 144.7(15) . . . . ? C33B C34B C37B C40B 78.4(15) . . . . ? C35B C34B C37B C40B -100.2(15) . . . . ? C21A C26A S1A C2 -111.2(8) . . . . ? C25A C26A S1A C2 76.2(9) . . . . ? C3 C2 S1A C26A -110.8(8) . . . . ? C1 C2 S1A C26A 68.7(9) . . . . ? S1B C2 S1A C26A 145(13) . . . . ? C11 C12 S2A C22A 121.2(5) . . . . ? C7 C12 S2A C22A -64.4(5) . . . . ? S2B C12 S2A C22A 57.7(19) . . . . ? C21A C22A S2A C12 114.6(5) . . . . ? C23A C22A S2A C12 -66.8(5) . . . . ? C9 C8 S3A C32A -130.0(5) . . . . ? C7 C8 S3A C32A 54.7(6) . . . . ? S3B C8 S3A C32A 109.8(11) . . . . ? C33A C32A S3A C8 69.2(5) . . . . ? C31A C32A S3A C8 -113.2(4) . . . . ? C31A C36A S4A C6 119.4(7) . . . . ? C35A C36A S4A C6 -58.6(7) . . . . ? C5 C6 S4A C36A 111.5(6) . . . . ? C1 C6 S4A C36A -67.8(8) . . . . ? S4B C6 S4A C36A -83(9) . . . . ? C3 C2 S1B C26B -109.6(14) . . . . ? C1 C2 S1B C26B 78.0(17) . . . . ? S1A C2 S1B C26B -30(11) . . . . ? C21B C26B S1B C2 -121(3) . . . . ? C25B C26B S1B C2 51(3) . . . . ? C21B C22B S2B C12 110(2) . . . . ? C23B C22B S2B C12 -65(2) . . . . ? C11 C12 S2B C22B 126.0(8) . . . . ? C7 C12 S2B C22B -44.5(9) . . . . ? S2A C12 S2B C22B -111(2) . . . . ? C9 C8 S3B C32B -123.6(8) . . . . ? C7 C8 S3B C32B 80.4(8) . . . . ? S3A C8 S3B C32B -52.9(10) . . . . ? C33B C32B S3B C8 59.6(9) . . . . ? C31B C32B S3B C8 -122.2(9) . . . . ? C5 C6 S4B C36B 102.5(13) . . . . ? C1 C6 S4B C36B -79.8(13) . . . . ? S4A C6 S4B C36B 86(9) . . . . ? C31B C36B S4B C6 120.4(12) . . . . ? C35B C36B S4B C6 -58.2(17) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.608 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.079 _database_code_depnum_ccdc_archive 'CCDC 974896' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5c_MeCN _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H53 N3 O2 S4' _chemical_formula_weight 760.11 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 Tetragonal _symmetry_space_group_name_H-M P4/ncc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-y, -x, -z+1/2' 'y+1/2, x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' 'y, x, z-1/2' '-y-1/2, -x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' _cell_length_a 15.3887(16) _cell_length_b 15.3887(16) _cell_length_c 17.563(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4159.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3362 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 21.90 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.266 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6023 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'phi and omega scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayered confocal mirror' _diffrn_measurement_device_type "Bruker APEX-II CCD'" _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21688 _diffrn_reflns_av_R_equivalents 0.0937 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2396 _reflns_number_gt 1447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)' _computing_publication_material ? _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^)+(0.1084P)^2^+4.7899P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2396 _refine_ls_number_parameters 159 _refine_ls_number_restraints 175 _refine_ls_R_factor_all 0.1247 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2528 _refine_ls_wR_factor_gt 0.2036 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2673(3) 0.0682(3) 0.3417(2) 0.0533(10) Uani 1 1 d U . . C2 C 0.3469(2) 0.0552(2) 0.3041(2) 0.0504(10) Uani 1 1 d D B . C3 C 0.3491(3) 0.0172(3) 0.2338(3) 0.0629(12) Uani 1 1 d . . . H19 H 0.4027 0.0101 0.2101 0.075 Uiso 1 1 calc R B . C4 C 0.2749(3) -0.0113(3) 0.1962(3) 0.0669(13) Uani 1 1 d . A . C5 C 0.1970(3) -0.0002(3) 0.2351(3) 0.0596(11) Uani 1 1 d . . . H20 H 0.1460 -0.0199 0.2125 0.072 Uiso 1 1 calc R B . C6 C 0.1918(2) 0.0383(2) 0.3048(2) 0.0506(10) Uani 1 1 d D B . C7 C 0.2787(3) -0.0545(4) 0.1181(4) 0.1001(17) Uani 1 1 d DU . . C8A C 0.3278(8) -0.1424(6) 0.1294(9) 0.106(3) Uani 0.50 1 d PDU A 1 H1 H 0.3315 -0.1723 0.0816 0.159 Uiso 0.50 1 calc PR A 1 H2 H 0.2967 -0.1777 0.1653 0.159 Uiso 0.50 1 calc PR A 1 H3 H 0.3852 -0.1312 0.1483 0.159 Uiso 0.50 1 calc PR A 1 C8B C 0.2795(14) -0.1533(6) 0.1305(12) 0.148(5) Uani 0.50 1 d PDU A 2 H4 H 0.2829 -0.1822 0.0821 0.222 Uiso 0.50 1 calc PR A 2 H5 H 0.2272 -0.1705 0.1562 0.222 Uiso 0.50 1 calc PR A 2 H6 H 0.3290 -0.1689 0.1608 0.222 Uiso 0.50 1 calc PR A 2 C9A C 0.1916(7) -0.0896(11) 0.0888(9) 0.117(4) Uani 0.50 1 d PDU A 1 H7 H 0.2002 -0.1172 0.0403 0.176 Uiso 0.50 1 calc PR A 1 H8 H 0.1512 -0.0425 0.0833 0.176 Uiso 0.50 1 calc PR A 1 H9 H 0.1690 -0.1312 0.1244 0.176 Uiso 0.50 1 calc PR A 1 C9B C 0.1979(6) -0.0242(10) 0.0715(7) 0.103(3) Uani 0.50 1 d PDU A 2 H10 H 0.1984 -0.0516 0.0223 0.155 Uiso 0.50 1 calc PR A 2 H11 H 0.1996 0.0377 0.0653 0.155 Uiso 0.50 1 calc PR A 2 H12 H 0.1458 -0.0402 0.0981 0.155 Uiso 0.50 1 calc PR A 2 C10B C 0.3558(10) -0.0263(11) 0.0688(12) 0.091(4) Uani 0.50 1 d PDU A 2 H13 H 0.3546 -0.0575 0.0215 0.136 Uiso 0.50 1 calc PR A 2 H14 H 0.4090 -0.0386 0.0951 0.136 Uiso 0.50 1 calc PR A 2 H15 H 0.3519 0.0350 0.0589 0.136 Uiso 0.50 1 calc PR A 2 C10A C 0.3400(12) 0.0006(11) 0.0687(12) 0.103(5) Uani 0.50 1 d PDU A 1 H16 H 0.3452 -0.0253 0.0192 0.154 Uiso 0.50 1 calc PR A 1 H17 H 0.3962 0.0032 0.0922 0.154 Uiso 0.50 1 calc PR A 1 H18 H 0.3169 0.0583 0.0637 0.154 Uiso 0.50 1 calc PR A 1 C12B C 0.225(2) 0.217(2) 0.1231(19) 0.072(7) Uiso 0.20 1 d P . 2 C12A C 0.2500 0.2500 0.122(4) 0.071(18) Uiso 0.20 4 d SP . 1 C11 C 0.2500 0.2500 0.1992(5) 0.065(2) Uiso 1 4 d S . . N2A N 0.2500 0.2500 0.058(6) 0.16(3) Uiso 0.20 4 d SP . 1 N2B N 0.1995(19) 0.2053(19) 0.0671(16) 0.100(7) Uiso 0.20 1 d P . 2 N1 N 0.2641(6) 0.0994(15) 0.4166(14) 0.073(4) Uani 0.50 1 d PDU B 1 O1 O 0.2609(5) 0.1195(11) 0.4034(11) 0.068(3) Uani 0.50 1 d PDU B 2 S1 S 0.44599(7) 0.08803(7) 0.34866(7) 0.0601(4) 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 C1 0.055(2) 0.044(2) 0.061(2) 0.0089(17) -0.0025(19) -0.0024(16) C2 0.043(2) 0.040(2) 0.068(3) 0.0049(19) -0.0117(19) 0.0019(15) C3 0.043(2) 0.065(3) 0.080(3) -0.009(2) -0.001(2) 0.0022(19) C4 0.050(3) 0.075(3) 0.075(3) -0.014(3) -0.005(2) 0.000(2) C5 0.046(2) 0.061(3) 0.072(3) 0.003(2) -0.011(2) -0.0049(19) C6 0.047(2) 0.039(2) 0.065(3) 0.0124(18) -0.0011(19) -0.0012(15) C7 0.082(3) 0.122(4) 0.096(4) -0.041(3) -0.004(3) -0.014(3) C8A 0.085(6) 0.112(5) 0.120(7) -0.049(5) -0.010(6) -0.018(4) C8B 0.160(8) 0.131(5) 0.153(8) -0.015(6) 0.014(6) -0.022(5) C9A 0.098(5) 0.141(8) 0.113(8) -0.046(7) -0.026(6) -0.010(5) C9B 0.082(5) 0.153(7) 0.076(6) -0.025(6) -0.002(5) -0.037(5) C10B 0.084(5) 0.101(7) 0.088(7) -0.027(6) -0.001(5) 0.016(6) C10A 0.094(8) 0.135(8) 0.080(7) -0.027(6) 0.010(6) 0.009(6) N1 0.093(7) 0.068(8) 0.058(6) 0.009(6) 0.004(5) -0.021(5) O1 0.074(5) 0.066(7) 0.064(7) -0.001(5) 0.004(4) -0.010(4) S1 0.0510(6) 0.0489(6) 0.0803(9) 0.0070(5) -0.0220(5) 0.0024(4) _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 C1 O1 1.35(2) . ? C1 N1 1.40(3) . ? C1 C2 1.406(6) . ? C1 C6 1.407(6) . ? C2 C3 1.367(6) . ? C2 S1 1.787(4) . ? C3 C4 1.390(6) . ? C3 H19 0.9300 . ? C4 C5 1.391(6) . ? C4 C7 1.526(8) . ? C5 C6 1.362(6) . ? C5 H20 0.9300 . ? C6 S1 1.790(4) 7 ? C7 C10B 1.530(6) . ? C7 C9A 1.534(6) . ? C7 C10A 1.536(6) . ? C7 C8B 1.536(6) . ? C7 C9B 1.560(6) . ? C7 C8A 1.562(6) . ? C8A H1 0.9600 . ? C8A H2 0.9600 . ? C8A H3 0.9600 . ? C8B H4 0.9600 . ? C8B H5 0.9600 . ? C8B H6 0.9600 . ? C9A H7 0.9600 . ? C9A H8 0.9600 . ? C9A H9 0.9600 . ? C9B H10 0.9600 . ? C9B H11 0.9600 . ? C9B H12 0.9600 . ? C10B H13 0.9600 . ? C10B H14 0.9600 . ? C10B H15 0.9600 . ? C10A H16 0.9600 . ? C10A H17 0.9600 . ? C10A H18 0.9600 . ? C12B C12B 0.89(4) 8 ? C12B C12B 0.89(4) 7 ? C12B N2B 1.08(4) . ? C12B C12B 1.26(6) 2 ? C12B N2B 1.48(5) 8 ? C12B C11 1.48(3) . ? C12B N2B 1.64(4) 7 ? C12B N2B 1.93(4) 2 ? C12A N2A 1.12(11) . ? C12A C11 1.35(8) . ? C11 C12B 1.48(3) 7 ? C11 C12B 1.48(3) 8 ? C11 C12B 1.48(3) 2 ? N2B N2B 1.47(4) 8 ? N2B N2B 1.47(4) 7 ? N2B C12B 1.48(5) 7 ? N2B C12B 1.64(4) 8 ? N2B C12B 1.93(4) 2 ? S1 C6 1.789(4) 8 ? 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 O1 C1 N1 16.2(14) . . ? O1 C1 C2 121.7(5) . . ? N1 C1 C2 121.3(5) . . ? O1 C1 C6 120.2(5) . . ? N1 C1 C6 121.0(5) . . ? C2 C1 C6 117.2(4) . . ? C3 C2 C1 120.4(4) . . ? C3 C2 S1 119.7(3) . . ? C1 C2 S1 119.9(3) . . ? C2 C3 C4 123.0(4) . . ? C2 C3 H19 118.5 . . ? C4 C3 H19 118.5 . . ? C3 C4 C5 115.8(4) . . ? C3 C4 C7 122.2(4) . . ? C5 C4 C7 121.9(4) . . ? C6 C5 C4 123.1(4) . . ? C6 C5 H20 118.5 . . ? C4 C5 H20 118.5 . . ? C5 C6 C1 120.5(4) . . ? C5 C6 S1 119.9(3) . 7 ? C1 C6 S1 119.6(3) . 7 ? C4 C7 C10B 114.5(9) . . ? C4 C7 C9A 114.9(7) . . ? C10B C7 C9A 126.0(12) . . ? C4 C7 C10A 106.9(10) . . ? C10B C7 C10A 18.0(11) . . ? C9A C7 C10A 122.8(12) . . ? C4 C7 C8B 107.7(9) . . ? C10B C7 C8B 110.8(11) . . ? C9A C7 C8B 72.8(10) . . ? C10A C7 C8B 128.4(12) . . ? C4 C7 C9B 108.1(6) . . ? C10B C7 C9B 103.7(11) . . ? C9A C7 C9B 39.9(7) . . ? C10A C7 C9B 91.7(11) . . ? C8B C7 C9B 112.1(10) . . ? C4 C7 C8A 106.3(7) . . ? C10B C7 C8A 86.8(9) . . ? C9A C7 C8A 99.2(9) . . ? C10A C7 C8A 104.7(10) . . ? C8B C7 C8A 28.4(8) . . ? C9B C7 C8A 135.3(8) . . ? C7 C8A H1 109.5 . . ? C7 C8A H2 109.5 . . ? H1 C8A H2 109.5 . . ? C7 C8A H3 109.5 . . ? H1 C8A H3 109.5 . . ? H2 C8A H3 109.5 . . ? C7 C8B H4 109.5 . . ? C7 C8B H5 109.5 . . ? H4 C8B H5 109.5 . . ? C7 C8B H6 109.5 . . ? H4 C8B H6 109.5 . . ? H5 C8B H6 109.5 . . ? C7 C9A H7 109.5 . . ? C7 C9A H8 109.5 . . ? H7 C9A H8 109.5 . . ? C7 C9A H9 109.5 . . ? H7 C9A H9 109.5 . . ? H8 C9A H9 109.5 . . ? C7 C9B H10 109.5 . . ? C7 C9B H11 109.5 . . ? H10 C9B H11 109.5 . . ? C7 C9B H12 109.5 . . ? H10 C9B H12 109.5 . . ? H11 C9B H12 109.5 . . ? C7 C10B H13 109.5 . . ? C7 C10B H14 109.5 . . ? H13 C10B H14 109.5 . . ? C7 C10B H15 109.5 . . ? H13 C10B H15 109.5 . . ? H14 C10B H15 109.5 . . ? C7 C10A H16 109.5 . . ? C7 C10A H17 109.5 . . ? H16 C10A H17 109.5 . . ? C7 C10A H18 109.5 . . ? H16 C10A H18 109.5 . . ? H17 C10A H18 109.5 . . ? C12B C12B C12B 89.999(15) 8 7 ? C12B C12B N2B 113(3) 8 . ? C12B C12B N2B 97(4) 7 . ? C12B C12B C12B 45.003(6) 8 2 ? C12B C12B C12B 44.996(2) 7 2 ? N2B C12B C12B 111(2) . 2 ? C12B C12B N2B 46(3) 8 8 ? C12B C12B N2B 107(2) 7 8 ? N2B C12B N2B 68(3) . 8 ? C12B C12B N2B 73(3) 2 8 ? C12B C12B C11 72.5(8) 8 . ? C12B C12B C11 72.5(8) 7 . ? N2B C12B C11 168(4) . . ? C12B C12B C11 64.8(11) 2 . ? N2B C12B C11 119(3) 8 . ? C12B C12B N2B 95(3) 8 7 ? C12B C12B N2B 37.1(18) 7 7 ? N2B C12B N2B 61(2) . 7 ? C12B C12B N2B 59(3) 2 7 ? N2B C12B N2B 83(2) 8 7 ? C11 C12B N2B 109(2) . 7 ? C12B C12B N2B 47(2) 8 2 ? C12B C12B N2B 58(2) 7 2 ? N2B C12B N2B 82(3) . 2 ? C12B C12B N2B 31.4(12) 2 2 ? N2B C12B N2B 48.9(14) 8 2 ? C11 C12B N2B 95.6(16) . 2 ? N2B C12B N2B 47.7(12) 7 2 ? N2A C12A C11 180.000(6) . . ? C12A C11 C12B 25.2(12) . . ? C12A C11 C12B 25.2(12) . 7 ? C12B C11 C12B 35.0(15) . 7 ? C12A C11 C12B 25.2(12) . 8 ? C12B C11 C12B 35.0(15) . 8 ? C12B C11 C12B 50(2) 7 8 ? C12A C11 C12B 25.2(12) . 2 ? C12B C11 C12B 50(2) . 2 ? C12B C11 C12B 35.0(15) 7 2 ? C12B C11 C12B 35.0(15) 8 2 ? C12B N2B N2B 69(3) . 8 ? C12B N2B N2B 79(2) . 7 ? N2B N2B N2B 90.002(2) 8 7 ? C12B N2B C12B 37(2) . 7 ? N2B N2B C12B 81.8(15) 8 7 ? N2B N2B C12B 42.9(15) 7 7 ? C12B N2B C12B 29.9(19) . 8 ? N2B N2B C12B 40.0(12) 8 8 ? N2B N2B C12B 76.4(15) 7 8 ? C12B N2B C12B 47(2) 7 8 ? C12B N2B C12B 37(2) . 2 ? N2B N2B C12B 55.9(14) 8 2 ? N2B N2B C12B 49.3(14) 7 2 ? C12B N2B C12B 26.2(12) 7 2 ? C12B N2B C12B 27.4(11) 8 2 ? C2 S1 C6 100.32(18) . 8 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -167.1(9) . . . . ? N1 C1 C2 C3 173.9(11) . . . . ? C6 C1 C2 C3 1.7(6) . . . . ? O1 C1 C2 S1 13.3(9) . . . . ? N1 C1 C2 S1 -5.7(11) . . . . ? C6 C1 C2 S1 -177.9(3) . . . . ? C1 C2 C3 C4 -0.7(7) . . . . ? S1 C2 C3 C4 178.9(4) . . . . ? C2 C3 C4 C5 -1.1(7) . . . . ? C2 C3 C4 C7 -179.3(5) . . . . ? C3 C4 C5 C6 1.8(7) . . . . ? C7 C4 C5 C6 -179.9(5) . . . . ? C4 C5 C6 C1 -0.8(7) . . . . ? C4 C5 C6 S1 177.2(4) . . . 7 ? O1 C1 C6 C5 168.0(9) . . . . ? N1 C1 C6 C5 -173.2(11) . . . . ? C2 C1 C6 C5 -1.0(6) . . . . ? O1 C1 C6 S1 -10.0(9) . . . 7 ? N1 C1 C6 S1 8.8(11) . . . 7 ? C2 C1 C6 S1 -179.1(3) . . . 7 ? C3 C4 C7 C10B -28.3(11) . . . . ? C5 C4 C7 C10B 153.6(9) . . . . ? C3 C4 C7 C9A 174.3(9) . . . . ? C5 C4 C7 C9A -3.9(11) . . . . ? C3 C4 C7 C10A -45.7(10) . . . . ? C5 C4 C7 C10A 136.1(9) . . . . ? C3 C4 C7 C8B 95.4(10) . . . . ? C5 C4 C7 C8B -82.8(10) . . . . ? C3 C4 C7 C9B -143.3(7) . . . . ? C5 C4 C7 C9B 38.6(8) . . . . ? C3 C4 C7 C8A 65.7(8) . . . . ? C5 C4 C7 C8A -112.5(7) . . . . ? N2A C12A C11 C12B 8(100) . . . . ? N2A C12A C11 C12B -82(100) . . . 7 ? N2A C12A C11 C12B 98(100) . . . 8 ? N2A C12A C11 C12B -172(100) . . . 2 ? C12B C12B C11 C12A 47.9(3) 8 . . . ? C12B C12B C11 C12A -47.9(3) 7 . . . ? N2B C12B C11 C12A -72(16) . . . . ? C12B C12B C11 C12A -0.002(9) 2 . . . ? N2B C12B C11 C12A 52(3) 8 . . . ? N2B C12B C11 C12A -41(3) 7 . . . ? N2B C12B C11 C12A 6(2) 2 . . . ? C12B C12B C11 C12B 95.7(5) 8 . . 7 ? N2B C12B C11 C12B -24(16) . . . 7 ? C12B C12B C11 C12B 47.8(3) 2 . . 7 ? N2B C12B C11 C12B 100(3) 8 . . 7 ? N2B C12B C11 C12B 7(3) 7 . . 7 ? N2B C12B C11 C12B 54(2) 2 . . 7 ? C12B C12B C11 C12B -95.7(5) 7 . . 8 ? N2B C12B C11 C12B -120(15) . . . 8 ? C12B C12B C11 C12B -47.9(3) 2 . . 8 ? N2B C12B C11 C12B 4(3) 8 . . 8 ? N2B C12B C11 C12B -89(2) 7 . . 8 ? N2B C12B C11 C12B -42(2) 2 . . 8 ? C12B C12B C11 C12B 47.9(3) 8 . . 2 ? C12B C12B C11 C12B -47.8(3) 7 . . 2 ? N2B C12B C11 C12B -72(16) . . . 2 ? N2B C12B C11 C12B 52(3) 8 . . 2 ? N2B C12B C11 C12B -41(3) 7 . . 2 ? N2B C12B C11 C12B 6(2) 2 . . 2 ? C12B C12B N2B N2B 12(5) 8 . . 8 ? C12B C12B N2B N2B 105(4) 7 . . 8 ? C12B C12B N2B N2B 61(5) 2 . . 8 ? C11 C12B N2B N2B 128(17) . . . 8 ? N2B C12B N2B N2B 94.4(10) 7 . . 8 ? N2B C12B N2B N2B 48.7(8) 2 . . 8 ? C12B C12B N2B N2B -82(5) 8 . . 7 ? C12B C12B N2B N2B 11(4) 7 . . 7 ? C12B C12B N2B N2B -34(5) 2 . . 7 ? N2B C12B N2B N2B -94.4(10) 8 . . 7 ? C11 C12B N2B N2B 34(16) . . . 7 ? N2B C12B N2B N2B -45.7(8) 2 . . 7 ? C12B C12B N2B C12B -93.0(15) 8 . . 7 ? C12B C12B N2B C12B -44.2(13) 2 . . 7 ? N2B C12B N2B C12B -105(4) 8 . . 7 ? C11 C12B N2B C12B 23(15) . . . 7 ? N2B C12B N2B C12B -11(4) 7 . . 7 ? N2B C12B N2B C12B -56(3) 2 . . 7 ? C12B C12B N2B C12B 93.0(15) 7 . . 8 ? C12B C12B N2B C12B 48.7(7) 2 . . 8 ? N2B C12B N2B C12B -12(5) 8 . . 8 ? C11 C12B N2B C12B 116(16) . . . 8 ? N2B C12B N2B C12B 82(5) 7 . . 8 ? N2B C12B N2B C12B 37(5) 2 . . 8 ? C12B C12B N2B C12B -48.7(7) 8 . . 2 ? C12B C12B N2B C12B 44.2(13) 7 . . 2 ? N2B C12B N2B C12B -61(5) 8 . . 2 ? C11 C12B N2B C12B 67(15) . . . 2 ? N2B C12B N2B C12B 34(5) 7 . . 2 ? N2B C12B N2B C12B -12(5) 2 . . 2 ? C3 C2 S1 C6 83.4(4) . . . 8 ? C1 C2 S1 C6 -97.0(3) . . . 8 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.491 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.065 _chemical_absolute_configuration ' ?' _database_code_depnum_ccdc_archive 'CCDC 974897' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_7c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H66 N2 O6 S4, C H4 O, H2 O' _chemical_formula_sum 'C57 H72 N2 O8 S4' _chemical_formula_weight 1041.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 13.8234(9) _cell_length_b 19.7567(10) _cell_length_c 24.5819(13) _cell_angle_alpha 90.00 _cell_angle_beta 123.419(3) _cell_angle_gamma 90.00 _cell_volume 5603.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 113 _cell_measurement_reflns_used 12380 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 0.223 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8200 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 113 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.6199 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44910 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9701 _reflns_number_gt 7721 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FS-PROCESS-AUTO(Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'FS-PROCESS-AUTO(Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996) and PLATON (Spek, 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita, 2001, Kabuto et al., 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9701 _refine_ls_number_parameters 849 _refine_ls_number_restraints 579 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1811 _refine_ls_wR_factor_gt 0.1695 _refine_ls_goodness_of_fit_ref 1.324 _refine_ls_restrained_S_all 1.307 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.36019(7) 0.77820(4) 0.29296(4) 0.0456(2) Uani 1 1 d . B . O1 O 0.4782(2) 0.79916(12) 0.34926(10) 0.0636(7) Uani 1 1 d . . . S2 S 0.08872(6) 0.92737(3) 0.05922(3) 0.03338(19) Uani 1 1 d . B . O2 O 0.04419(17) 0.97176(10) 0.09048(10) 0.0432(5) Uani 1 1 d . . . S3 S -0.08340(6) 0.68935(4) -0.08752(3) 0.0378(2) Uani 1 1 d . . . O3 O -0.06352(19) 0.71914(11) -0.13634(9) 0.0486(5) Uani 1 1 d . . . S4 S 0.19057(6) 0.54672(4) 0.14178(4) 0.0440(2) Uani 1 1 d . D . O4 O 0.2419(2) 0.47844(11) 0.14675(11) 0.0587(6) Uani 1 1 d . . . C1 C 0.1012(3) 0.6749(2) 0.2011(2) 0.0720(11) Uani 1 1 d . . . H1 H 0.0736 0.6284 0.1874 0.108 Uiso 1 1 calc R . . H1A H 0.0354 0.7062 0.1790 0.108 Uiso 1 1 calc R . . H1B H 0.1389 0.6788 0.2483 0.108 Uiso 1 1 calc R . . O5 O 0.18124(19) 0.69110(12) 0.18468(12) 0.0599(6) Uani 1 1 d . . . C2 C 0.2886(2) 0.66130(14) 0.21828(13) 0.0385(7) Uani 1 1 d . B . C3 C 0.3087(2) 0.59870(15) 0.20167(13) 0.0390(6) Uani 1 1 d . . . C4 C 0.4216(3) 0.57348(14) 0.23114(14) 0.0405(7) Uani 1 1 d . B . H4 H 0.4333 0.5302 0.2189 0.049 Uiso 1 1 calc R . . C5 C 0.5159(2) 0.61051(15) 0.27772(14) 0.0426(7) Uani 1 1 d . . . C6 C 0.4948(3) 0.67279(15) 0.29696(14) 0.0432(7) Uani 1 1 d . B . H6 H 0.5579 0.6982 0.3307 0.052 Uiso 1 1 calc R . . C7 C 0.3835(3) 0.69750(14) 0.26744(13) 0.0386(7) Uani 1 1 d . . . N1 N 0.1383(2) 0.86943(12) 0.18952(11) 0.0389(6) Uani 1 1 d . A . H1C H 0.0678 0.8757 0.1549 0.047 Uiso 1 1 calc R . . C8 C 0.2257(2) 0.85893(12) 0.17959(13) 0.0313(6) Uani 1 1 d . A . C9 C 0.3315(2) 0.82523(13) 0.22319(13) 0.0349(6) Uani 1 1 d . . . C10 C 0.4201(2) 0.82417(15) 0.21254(14) 0.0398(7) Uani 1 1 d . B . H10 H 0.4910 0.8031 0.2444 0.048 Uiso 1 1 calc R . . C11 C 0.4117(2) 0.85159(15) 0.15896(14) 0.0386(7) Uani 1 1 d . . . C12 C 0.3035(2) 0.88036(14) 0.11261(13) 0.0356(6) Uani 1 1 d . B . H12 H 0.2913 0.8979 0.0733 0.043 Uiso 1 1 calc R . . C13 C 0.2150(2) 0.88376(13) 0.12254(13) 0.0319(6) Uani 1 1 d . . . N2 N 0.08384(19) 0.81930(12) -0.02807(11) 0.0366(5) Uani 1 1 d . . . H2 H 0.1485 0.7957 -0.0083 0.044 Uiso 1 1 calc R . . C14 C -0.0015(2) 0.81009(13) -0.01426(12) 0.0308(6) Uani 1 1 d . B . C15 C -0.0796(2) 0.75563(13) -0.03637(12) 0.0326(6) Uani 1 1 d . . . C16 C -0.1608(2) 0.74954(14) -0.02038(13) 0.0357(6) Uani 1 1 d . C . H16 H -0.2120 0.7119 -0.0365 0.043 Uiso 1 1 calc R . . C17 C -0.1702(2) 0.79650(15) 0.01837(13) 0.0375(6) Uani 1 1 d . . . C18 C -0.0943(2) 0.85131(14) 0.03966(13) 0.0352(6) Uani 1 1 d . B . H18 H -0.0994 0.8856 0.0651 0.042 Uiso 1 1 calc R . . C19 C -0.0118(2) 0.85709(13) 0.02469(12) 0.0317(6) Uani 1 1 d . . . C20 C -0.0944(3) 0.56740(18) 0.0217(2) 0.0671(10) Uani 1 1 d . . . H20 H -0.1349 0.5597 -0.0253 0.101 Uiso 1 1 calc R . . H20A H -0.1511 0.5763 0.0329 0.101 Uiso 1 1 calc R . . H20B H -0.0489 0.5272 0.0452 0.101 Uiso 1 1 calc R . . O6 O -0.01864(17) 0.62442(10) 0.03978(10) 0.0423(5) Uani 1 1 d . . . C21 C 0.0661(2) 0.61839(13) 0.02699(13) 0.0351(6) Uani 1 1 d . D . C22 C 0.0514(2) 0.64763(14) -0.02834(13) 0.0358(6) Uani 1 1 d . . . C23 C 0.1356(3) 0.64177(14) -0.04240(14) 0.0406(7) Uani 1 1 d . D . H23 H 0.1220 0.6607 -0.0816 0.049 Uiso 1 1 calc R . . C24 C 0.2404(3) 0.60832(15) 0.00049(14) 0.0419(7) Uani 1 1 d . . . C25 C 0.2562(3) 0.58090(15) 0.05691(15) 0.0422(7) Uani 1 1 d . D . H25 H 0.3265 0.5580 0.0869 0.051 Uiso 1 1 calc R . . C26 C 0.1710(2) 0.58632(14) 0.07036(14) 0.0372(6) Uani 1 1 d . . . C27 C 0.0583(3) 0.87103(16) -0.07791(15) 0.0436(7) Uani 1 1 d . . . H27 H 0.0310 0.9130 -0.0685 0.052 Uiso 1 1 calc R . . H27A H -0.0045 0.8545 -0.1214 0.052 Uiso 1 1 calc R . . C28 C 0.1639(3) 0.88637(16) -0.07877(14) 0.0429(7) Uani 1 1 d . . . C29 C 0.2193(3) 0.94813(18) -0.05765(19) 0.0587(9) Uani 1 1 d . . . H29 H 0.1918 0.9808 -0.0409 0.070 Uiso 1 1 calc R . . C30 C 0.3144(4) 0.9630(2) -0.0605(2) 0.0763(12) Uani 1 1 d . . . H30 H 0.3507 1.0061 -0.0466 0.092 Uiso 1 1 calc R . . C31 C 0.3559(4) 0.9159(3) -0.0833(2) 0.0777(13) Uani 1 1 d . . . H31 H 0.4217 0.9260 -0.0847 0.093 Uiso 1 1 calc R . . C32 C 0.3027(4) 0.8539(2) -0.1043(2) 0.0702(11) Uani 1 1 d . . . H32 H 0.3317 0.8212 -0.1202 0.084 Uiso 1 1 calc R . . C33 C 0.2068(3) 0.83918(19) -0.10226(17) 0.0562(9) Uani 1 1 d . . . H33 H 0.1699 0.7964 -0.1171 0.067 Uiso 1 1 calc R . . C35A C 0.0590(8) 0.9125(6) 0.2486(6) 0.041(2) Uani 0.50 1 d PGU A 1 C36A C 0.0041(10) 0.8793(5) 0.2742(7) 0.052(2) Uani 0.50 1 d PGU A 1 H36A H 0.0297 0.8356 0.2930 0.062 Uiso 0.50 1 calc PR A 1 C37A C -0.0883(9) 0.9099(5) 0.2723(6) 0.056(2) Uani 0.50 1 d PGU A 1 H37A H -0.1258 0.8871 0.2898 0.067 Uiso 0.50 1 calc PR A 1 C38A C -0.1257(7) 0.9737(4) 0.2448(5) 0.051(2) Uani 0.50 1 d PGU A 1 H38A H -0.1888 0.9947 0.2435 0.061 Uiso 0.50 1 calc PR A 1 C39A C -0.0707(6) 1.0070(4) 0.2191(5) 0.052(2) Uani 0.50 1 d PGU A 1 H39A H -0.0963 1.0507 0.2003 0.062 Uiso 0.50 1 calc PR A 1 C40A C 0.0216(7) 0.9764(6) 0.2211(5) 0.051(2) Uani 0.50 1 d PGU A 1 H40A H 0.0592 0.9992 0.2036 0.061 Uiso 0.50 1 calc PR A 1 C35B C 0.0599(8) 0.9112(6) 0.2534(6) 0.046(2) Uani 0.50 1 d PGU A 2 C36B C -0.0140(10) 0.8853(5) 0.2700(6) 0.0427(18) Uani 0.50 1 d PGU A 2 H36B H -0.0078 0.8392 0.2826 0.051 Uiso 0.50 1 calc PR A 2 C37B C -0.0970(9) 0.9267(5) 0.2681(6) 0.051(2) Uani 0.50 1 d PGU A 2 H37B H -0.1475 0.9090 0.2795 0.061 Uiso 0.50 1 calc PR A 2 C38B C -0.1062(7) 0.9941(4) 0.2497(5) 0.057(2) Uani 0.50 1 d PGU A 2 H38B H -0.1629 1.0225 0.2484 0.069 Uiso 0.50 1 calc PR A 2 C39B C -0.0323(7) 1.0201(5) 0.2330(5) 0.056(2) Uani 0.50 1 d PGU A 2 H39B H -0.0385 1.0661 0.2204 0.067 Uiso 0.50 1 calc PR A 2 C40B C 0.0507(7) 0.9786(6) 0.2349(5) 0.0498(19) Uani 0.50 1 d PGU A 2 H40B H 0.1012 0.9963 0.2235 0.060 Uiso 0.50 1 calc PR A 2 C41A C 0.6422(14) 0.5862(8) 0.3042(7) 0.050(3) Uani 0.50 1 d PDU B 1 C42A C 0.647(3) 0.5188(9) 0.2747(10) 0.050(3) Uani 0.50 1 d PDU B 1 H34J H 0.6036 0.4843 0.2817 0.074 Uiso 0.50 1 calc PR B 1 H34K H 0.7275 0.5044 0.2957 0.074 Uiso 0.50 1 calc PR B 1 H34L H 0.6117 0.5245 0.2279 0.074 Uiso 0.50 1 calc PR B 1 C43A C 0.7084(15) 0.5787(9) 0.3792(7) 0.066(4) Uani 0.50 1 d PDU B 1 H43A H 0.7023 0.6209 0.3981 0.099 Uiso 0.50 1 calc PR B 1 H43B H 0.7902 0.5689 0.3972 0.099 Uiso 0.50 1 calc PR B 1 H43C H 0.6746 0.5416 0.3899 0.099 Uiso 0.50 1 calc PR B 1 C44A C 0.6994(13) 0.6409(7) 0.2870(6) 0.068(3) Uani 0.50 1 d PDU B 1 H44A H 0.6552 0.6468 0.2396 0.102 Uiso 0.50 1 calc PR B 1 H44B H 0.7789 0.6273 0.3029 0.102 Uiso 0.50 1 calc PR B 1 H44C H 0.7008 0.6837 0.3076 0.102 Uiso 0.50 1 calc PR B 1 C41B C 0.6387(15) 0.5882(8) 0.3103(7) 0.057(3) Uani 0.50 1 d PDU B 2 C42B C 0.646(3) 0.5308(10) 0.2708(12) 0.065(5) Uani 0.50 1 d PDU B 2 H42B H 0.6061 0.4908 0.2726 0.098 Uiso 0.50 1 calc PR B 2 H42C H 0.7276 0.5198 0.2892 0.098 Uiso 0.50 1 calc PR B 2 H42D H 0.6093 0.5452 0.2254 0.098 Uiso 0.50 1 calc PR B 2 C43B C 0.6821(16) 0.5620(9) 0.3797(7) 0.069(4) Uani 0.50 1 d PDU B 2 H43D H 0.6764 0.5984 0.4049 0.103 Uiso 0.50 1 calc PR B 2 H43E H 0.7630 0.5475 0.4015 0.103 Uiso 0.50 1 calc PR B 2 H43F H 0.6342 0.5237 0.3764 0.103 Uiso 0.50 1 calc PR B 2 C44B C 0.7170(13) 0.6462(8) 0.3156(6) 0.081(4) Uani 0.50 1 d PDU B 2 H44D H 0.6897 0.6630 0.2719 0.121 Uiso 0.50 1 calc PR B 2 H44E H 0.7967 0.6297 0.3367 0.121 Uiso 0.50 1 calc PR B 2 H44F H 0.7146 0.6829 0.3416 0.121 Uiso 0.50 1 calc PR B 2 C45A C 0.5088(11) 0.8486(6) 0.1471(5) 0.055(2) Uani 0.50 1 d PDU B 1 C46A C 0.4794(11) 0.7922(5) 0.0974(5) 0.077(3) Uani 0.50 1 d PDU B 1 H46A H 0.4828 0.7482 0.1169 0.115 Uiso 0.50 1 calc PR B 1 H46B H 0.5354 0.7928 0.0848 0.115 Uiso 0.50 1 calc PR B 1 H46C H 0.4012 0.7994 0.0587 0.115 Uiso 0.50 1 calc PR B 1 C47A C 0.6270(12) 0.8367(6) 0.2115(5) 0.067(3) Uani 0.50 1 d PDU B 1 H47A H 0.6455 0.8754 0.2406 0.100 Uiso 0.50 1 calc PR B 1 H47B H 0.6873 0.8317 0.2024 0.100 Uiso 0.50 1 calc PR B 1 H47C H 0.6233 0.7955 0.2325 0.100 Uiso 0.50 1 calc PR B 1 C48A C 0.5184(11) 0.9161(6) 0.1185(5) 0.074(3) Uani 0.50 1 d PDU B 1 H48A H 0.4506 0.9215 0.0738 0.111 Uiso 0.50 1 calc PR B 1 H48B H 0.5889 0.9158 0.1181 0.111 Uiso 0.50 1 calc PR B 1 H48C H 0.5218 0.9539 0.1453 0.111 Uiso 0.50 1 calc PR B 1 C45B C 0.5087(11) 0.8490(6) 0.1462(5) 0.055(2) Uani 0.50 1 d PDU B 2 C46B C 0.4578(10) 0.8147(5) 0.0797(5) 0.069(2) Uani 0.50 1 d PDU B 2 H46D H 0.5208 0.8017 0.0746 0.104 Uiso 0.50 1 calc PR B 2 H46E H 0.4057 0.8463 0.0449 0.104 Uiso 0.50 1 calc PR B 2 H46F H 0.4145 0.7742 0.0771 0.104 Uiso 0.50 1 calc PR B 2 C47B C 0.6163(11) 0.8108(5) 0.2006(5) 0.063(2) Uani 0.50 1 d PDU B 2 H47D H 0.6783 0.8134 0.1926 0.095 Uiso 0.50 1 calc PR B 2 H47E H 0.5962 0.7633 0.2009 0.095 Uiso 0.50 1 calc PR B 2 H47F H 0.6427 0.8315 0.2428 0.095 Uiso 0.50 1 calc PR B 2 C48B C 0.5460(11) 0.9221(5) 0.1431(5) 0.071(3) Uani 0.50 1 d PDU B 2 H48D H 0.5777 0.9443 0.1853 0.107 Uiso 0.50 1 calc PR B 2 H48E H 0.4787 0.9475 0.1091 0.107 Uiso 0.50 1 calc PR B 2 H48F H 0.6054 0.9206 0.1330 0.107 Uiso 0.50 1 calc PR B 2 C49A C -0.2606(10) 0.7904(6) 0.0362(7) 0.0512(19) Uani 0.50 1 d PDU C 1 C50A C -0.1994(13) 0.8035(6) 0.1094(6) 0.063(3) Uani 0.50 1 d PDU C 1 H50A H -0.1383 0.7697 0.1337 0.094 Uiso 0.50 1 calc PR C 1 H50B H -0.2557 0.8003 0.1217 0.094 Uiso 0.50 1 calc PR C 1 H50C H -0.1651 0.8489 0.1197 0.094 Uiso 0.50 1 calc PR C 1 C51A C -0.3184(8) 0.7220(5) 0.0199(5) 0.066(2) Uani 0.50 1 d PDU C 1 H34G H -0.3663 0.7161 -0.0275 0.099 Uiso 0.50 1 calc PR C 1 H34H H -0.3674 0.7189 0.0372 0.099 Uiso 0.50 1 calc PR C 1 H34I H -0.2592 0.6865 0.0395 0.099 Uiso 0.50 1 calc PR C 1 C52A C -0.3575(9) 0.8432(5) -0.0043(5) 0.062(2) Uani 0.50 1 d PDU C 1 H52A H -0.3240 0.8888 0.0064 0.093 Uiso 0.50 1 calc PR C 1 H52B H -0.4163 0.8398 0.0061 0.093 Uiso 0.50 1 calc PR C 1 H52C H -0.3934 0.8345 -0.0508 0.093 Uiso 0.50 1 calc PR C 1 C49B C -0.2563(10) 0.7876(6) 0.0389(6) 0.0513(19) Uani 0.50 1 d PDU C 2 C50B C -0.2717(9) 0.7118(5) 0.0467(5) 0.066(2) Uani 0.50 1 d PDU C 2 H50D H -0.3267 0.7064 0.0598 0.098 Uiso 0.50 1 calc PR C 2 H50E H -0.1967 0.6923 0.0802 0.098 Uiso 0.50 1 calc PR C 2 H50F H -0.3014 0.6885 0.0052 0.098 Uiso 0.50 1 calc PR C 2 C51B C -0.3739(9) 0.8129(5) -0.0141(5) 0.069(2) Uani 0.50 1 d PDU C 2 H51B H -0.4067 0.7827 -0.0519 0.103 Uiso 0.50 1 calc PR C 2 H51C H -0.3668 0.8587 -0.0268 0.103 Uiso 0.50 1 calc PR C 2 H51D H -0.4249 0.8138 0.0020 0.103 Uiso 0.50 1 calc PR C 2 C52B C -0.2141(13) 0.8264(6) 0.1028(6) 0.060(2) Uani 0.50 1 d PDU C 2 H52D H -0.2175 0.8752 0.0948 0.089 Uiso 0.50 1 calc PR C 2 H52E H -0.1341 0.8133 0.1359 0.089 Uiso 0.50 1 calc PR C 2 H52F H -0.2640 0.8153 0.1184 0.089 Uiso 0.50 1 calc PR C 2 C53A C 0.3295(10) 0.5984(6) -0.0199(6) 0.050(2) Uani 0.65(4) 1 d PDU D 1 C54A C 0.3400(18) 0.6629(7) -0.0519(9) 0.067(4) Uani 0.65(4) 1 d PDU D 1 H54A H 0.4028 0.6571 -0.0588 0.101 Uiso 0.65(4) 1 calc PR D 1 H54B H 0.3568 0.7018 -0.0232 0.101 Uiso 0.65(4) 1 calc PR D 1 H54C H 0.2669 0.6707 -0.0938 0.101 Uiso 0.65(4) 1 calc PR D 1 C55A C 0.2866(14) 0.5391(6) -0.0682(9) 0.064(3) Uani 0.65(4) 1 d PDU D 1 H34D H 0.2106 0.5502 -0.1071 0.096 Uiso 0.65(4) 1 calc PR D 1 H34E H 0.2800 0.4984 -0.0476 0.096 Uiso 0.65(4) 1 calc PR D 1 H34F H 0.3418 0.5307 -0.0806 0.096 Uiso 0.65(4) 1 calc PR D 1 C56A C 0.4517(12) 0.5822(10) 0.0404(7) 0.070(3) Uani 0.65(4) 1 d PDU D 1 H56A H 0.4497 0.5387 0.0590 0.105 Uiso 0.65(4) 1 calc PR D 1 H56B H 0.4756 0.6180 0.0731 0.105 Uiso 0.65(4) 1 calc PR D 1 H56C H 0.5070 0.5796 0.0274 0.105 Uiso 0.65(4) 1 calc PR D 1 C53B C 0.332(2) 0.5980(10) -0.0125(12) 0.052(4) Uani 0.35(4) 1 d PDU D 2 C54B C 0.323(3) 0.6543(12) -0.0586(14) 0.055(4) Uani 0.35(4) 1 d PDU D 2 H54D H 0.2487 0.6508 -0.1006 0.083 Uiso 0.35(4) 1 calc PR D 2 H54E H 0.3865 0.6493 -0.0652 0.083 Uiso 0.35(4) 1 calc PR D 2 H54F H 0.3288 0.6987 -0.0391 0.083 Uiso 0.35(4) 1 calc PR D 2 C55B C 0.316(3) 0.5289(11) -0.0451(16) 0.065(4) Uani 0.35(4) 1 d PDU D 2 H55B H 0.3387 0.4928 -0.0128 0.097 Uiso 0.35(4) 1 calc PR D 2 H55C H 0.3639 0.5266 -0.0630 0.097 Uiso 0.35(4) 1 calc PR D 2 H55D H 0.2341 0.5230 -0.0804 0.097 Uiso 0.35(4) 1 calc PR D 2 C56B C 0.455(2) 0.6027(15) 0.0510(11) 0.062(4) Uani 0.35(4) 1 d PDU D 2 H56D H 0.4604 0.6442 0.0745 0.093 Uiso 0.35(4) 1 calc PR D 2 H56E H 0.5129 0.6036 0.0402 0.093 Uiso 0.35(4) 1 calc PR D 2 H56F H 0.4679 0.5633 0.0786 0.093 Uiso 0.35(4) 1 calc PR D 2 C1S C 0.8422(11) 0.6593(7) 0.2144(6) 0.235(5) Uani 1 1 d . . . H1S H 0.7648 0.6769 0.1985 0.353 Uiso 1 1 calc R . . H2S H 0.8539 0.6165 0.2374 0.353 Uiso 1 1 calc R . . H3S H 0.8494 0.6516 0.1774 0.353 Uiso 1 1 calc R . . O1S O 0.9260(8) 0.7062(5) 0.2571(4) 0.231(3) Uani 1 1 d . . . H4S H 0.9059 0.7234 0.2806 0.346 Uiso 1 1 calc R . . O1W O 0.3914(5) 0.4234(3) 0.1066(3) 0.159(2) Uani 1 1 d D . . H1W H 0.371(6) 0.432(4) 0.133(3) 0.191 Uiso 1 1 d D . . H2W H 0.448(5) 0.395(3) 0.128(3) 0.191 Uiso 1 1 d D . . C34 C 0.1536(3) 0.87100(17) 0.25331(15) 0.0478(8) Uani 1 1 d . . . H34 H 0.2300 0.8909 0.2860 0.072 Uiso 0.50 1 calc PR A 1 H34A H 0.1510 0.8244 0.2673 0.072 Uiso 0.50 1 calc PR A 1 H34B H 0.2301 0.8912 0.2854 0.072 Uiso 0.50 1 calc PR A 2 H34C H 0.1535 0.8240 0.2673 0.072 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0611(5) 0.0436(4) 0.0386(4) 0.0078(3) 0.0316(4) 0.0146(4) O1 0.0770(17) 0.0549(14) 0.0332(12) -0.0035(10) 0.0142(12) 0.0116(12) S2 0.0308(4) 0.0317(4) 0.0364(4) 0.0025(3) 0.0178(3) 0.0026(3) O2 0.0413(11) 0.0363(11) 0.0490(12) -0.0035(9) 0.0231(10) 0.0061(9) S3 0.0345(4) 0.0426(4) 0.0315(4) -0.0051(3) 0.0152(3) 0.0055(3) O3 0.0558(13) 0.0567(13) 0.0354(11) 0.0051(9) 0.0265(10) 0.0164(10) S4 0.0388(4) 0.0455(4) 0.0398(4) 0.0057(3) 0.0167(3) -0.0066(3) O4 0.0634(15) 0.0378(12) 0.0579(14) 0.0037(10) 0.0228(12) -0.0043(10) C1 0.051(2) 0.089(3) 0.089(3) 0.000(2) 0.047(2) 0.001(2) O5 0.0374(12) 0.0683(15) 0.0732(16) 0.0254(12) 0.0300(12) 0.0140(11) C2 0.0362(16) 0.0438(17) 0.0380(15) 0.0131(13) 0.0219(13) 0.0074(12) C3 0.0343(15) 0.0463(17) 0.0302(14) 0.0045(12) 0.0138(12) -0.0028(12) C4 0.0398(16) 0.0351(15) 0.0405(16) 0.0038(12) 0.0182(14) 0.0031(12) C5 0.0353(16) 0.0417(16) 0.0404(16) 0.0035(13) 0.0144(13) 0.0067(12) C6 0.0410(17) 0.0430(17) 0.0333(15) 0.0029(12) 0.0128(13) 0.0058(13) C7 0.0448(17) 0.0380(15) 0.0337(15) 0.0068(12) 0.0221(13) 0.0093(12) N1 0.0331(13) 0.0521(15) 0.0343(12) -0.0025(11) 0.0205(11) 0.0031(10) C8 0.0347(15) 0.0282(13) 0.0351(14) -0.0019(11) 0.0218(12) -0.0002(11) C9 0.0392(16) 0.0339(14) 0.0331(14) 0.0027(11) 0.0210(13) 0.0050(12) C10 0.0338(15) 0.0449(16) 0.0404(16) 0.0029(13) 0.0202(13) 0.0095(12) C11 0.0319(15) 0.0444(16) 0.0415(16) 0.0015(13) 0.0214(13) 0.0043(12) C12 0.0329(15) 0.0406(16) 0.0361(15) -0.0002(12) 0.0209(13) -0.0010(11) C13 0.0281(14) 0.0314(14) 0.0330(14) -0.0001(11) 0.0149(12) -0.0002(10) N2 0.0290(12) 0.0433(13) 0.0431(13) 0.0080(10) 0.0234(11) 0.0092(10) C14 0.0272(13) 0.0363(14) 0.0293(14) 0.0047(11) 0.0158(11) 0.0078(11) C15 0.0294(14) 0.0360(14) 0.0292(14) -0.0005(11) 0.0141(12) 0.0053(11) C16 0.0289(14) 0.0407(15) 0.0358(15) -0.0039(12) 0.0168(12) -0.0020(12) C17 0.0287(14) 0.0492(17) 0.0348(15) -0.0009(12) 0.0175(12) 0.0027(12) C18 0.0292(14) 0.0442(16) 0.0351(15) -0.0046(12) 0.0195(12) 0.0019(12) C19 0.0267(13) 0.0361(14) 0.0295(13) 0.0011(11) 0.0136(11) 0.0022(11) C20 0.049(2) 0.056(2) 0.097(3) -0.015(2) 0.041(2) -0.0180(17) O6 0.0399(11) 0.0414(11) 0.0547(12) -0.0020(9) 0.0317(10) -0.0024(9) C21 0.0357(15) 0.0311(14) 0.0379(15) -0.0058(11) 0.0200(13) -0.0037(11) C22 0.0326(15) 0.0373(15) 0.0337(15) -0.0037(11) 0.0158(12) 0.0031(11) C23 0.0429(17) 0.0422(16) 0.0399(16) 0.0009(13) 0.0247(14) 0.0091(13) C24 0.0376(16) 0.0440(16) 0.0445(17) -0.0032(13) 0.0229(14) 0.0042(13) C25 0.0337(15) 0.0447(17) 0.0441(17) 0.0052(13) 0.0187(14) 0.0046(12) C26 0.0358(15) 0.0343(15) 0.0377(15) 0.0018(12) 0.0179(13) -0.0016(12) C27 0.0375(16) 0.0589(19) 0.0402(16) 0.0089(14) 0.0250(14) 0.0092(14) C28 0.0443(17) 0.0532(18) 0.0406(16) 0.0167(14) 0.0292(14) 0.0138(14) C29 0.064(2) 0.049(2) 0.071(2) 0.0081(17) 0.042(2) 0.0022(16) C30 0.066(3) 0.069(3) 0.103(3) 0.020(2) 0.052(3) -0.002(2) C31 0.059(2) 0.100(3) 0.092(3) 0.041(3) 0.053(2) 0.017(2) C32 0.072(3) 0.091(3) 0.075(3) 0.022(2) 0.058(2) 0.029(2) C33 0.065(2) 0.061(2) 0.062(2) 0.0096(17) 0.0470(19) 0.0138(17) C35A 0.051(3) 0.053(3) 0.036(3) 0.001(3) 0.034(3) 0.006(3) C36A 0.046(4) 0.061(4) 0.052(3) 0.003(3) 0.028(3) 0.010(3) C37A 0.051(4) 0.066(5) 0.054(3) 0.013(3) 0.030(3) 0.005(3) C38A 0.054(3) 0.060(5) 0.051(3) 0.002(3) 0.037(3) 0.013(3) C39A 0.056(4) 0.054(4) 0.050(4) 0.005(3) 0.032(3) 0.015(3) C40A 0.057(4) 0.058(3) 0.047(4) 0.006(3) 0.035(3) 0.011(3) C35B 0.051(3) 0.051(3) 0.041(3) 0.003(3) 0.029(3) 0.008(3) C36B 0.038(3) 0.055(3) 0.048(3) 0.004(3) 0.032(3) 0.009(3) C37B 0.048(3) 0.061(5) 0.059(3) 0.002(3) 0.040(3) 0.011(3) C38B 0.063(4) 0.059(5) 0.057(4) 0.003(4) 0.038(3) 0.016(4) C39B 0.063(5) 0.059(4) 0.057(4) 0.006(3) 0.039(4) 0.013(4) C40B 0.054(4) 0.062(3) 0.048(4) 0.005(3) 0.038(3) 0.012(3) C41A 0.032(4) 0.044(4) 0.061(4) -0.002(4) 0.017(3) 0.009(3) C42A 0.051(6) 0.043(6) 0.051(5) 0.007(5) 0.026(4) 0.021(5) C43A 0.037(6) 0.056(7) 0.060(5) -0.010(5) -0.002(4) 0.006(5) C44A 0.035(6) 0.065(5) 0.090(7) -0.002(6) 0.025(6) 0.005(4) C41B 0.039(4) 0.043(4) 0.064(5) -0.002(4) 0.012(4) 0.007(4) C42B 0.046(6) 0.058(8) 0.077(7) 0.010(6) 0.025(5) 0.019(7) C43B 0.050(8) 0.057(8) 0.052(5) -0.010(4) -0.001(5) 0.019(5) C44B 0.028(4) 0.069(6) 0.101(9) -0.004(7) 0.007(6) 0.001(4) C45A 0.038(3) 0.081(3) 0.060(3) 0.010(3) 0.035(2) 0.010(2) C46A 0.058(4) 0.103(5) 0.076(5) -0.008(4) 0.042(4) 0.021(4) C47A 0.040(4) 0.090(5) 0.076(4) 0.003(4) 0.035(3) 0.007(4) C48A 0.047(5) 0.106(5) 0.074(5) 0.026(4) 0.037(4) -0.001(4) C45B 0.038(2) 0.081(3) 0.060(3) 0.010(3) 0.036(2) 0.010(2) C46B 0.056(4) 0.099(5) 0.067(4) 0.006(4) 0.044(3) 0.023(4) C47B 0.036(4) 0.090(5) 0.071(4) 0.008(4) 0.034(3) 0.019(4) C48B 0.042(5) 0.099(4) 0.071(5) 0.019(4) 0.030(4) -0.004(4) C49A 0.041(3) 0.072(3) 0.056(3) -0.014(2) 0.036(2) -0.011(2) C50A 0.057(4) 0.085(6) 0.057(4) -0.006(4) 0.038(3) -0.012(4) C51A 0.050(4) 0.087(4) 0.070(5) -0.011(4) 0.038(3) -0.016(4) C52A 0.040(4) 0.089(5) 0.070(4) 0.001(4) 0.038(3) 0.003(4) C49B 0.040(3) 0.072(3) 0.056(3) -0.015(3) 0.036(2) -0.010(2) C50B 0.061(5) 0.083(4) 0.077(5) -0.010(4) 0.053(4) -0.015(4) C51B 0.037(3) 0.104(6) 0.069(4) -0.010(4) 0.032(3) -0.010(4) C52B 0.054(4) 0.085(6) 0.058(4) -0.014(4) 0.043(3) -0.015(4) C53A 0.046(3) 0.058(3) 0.060(4) 0.007(3) 0.038(3) 0.015(3) C54A 0.063(7) 0.073(6) 0.079(6) 0.016(5) 0.048(5) 0.007(4) C55A 0.072(6) 0.066(5) 0.068(6) 0.006(4) 0.048(5) 0.020(4) C56A 0.049(4) 0.087(7) 0.078(5) 0.008(5) 0.038(4) 0.024(5) C53B 0.053(5) 0.054(5) 0.064(5) 0.008(5) 0.042(4) 0.007(5) C54B 0.044(7) 0.068(8) 0.081(8) 0.001(7) 0.051(6) 0.004(6) C55B 0.064(9) 0.076(8) 0.070(10) -0.002(7) 0.046(7) 0.019(7) C56B 0.044(6) 0.076(9) 0.084(8) 0.019(7) 0.046(6) 0.025(7) C1S 0.256(14) 0.204(11) 0.215(12) -0.030(10) 0.111(11) -0.044(10) O1S 0.277(9) 0.270(9) 0.206(7) -0.032(7) 0.171(7) -0.024(8) O1W 0.188(5) 0.149(4) 0.171(5) 0.067(3) 0.119(4) 0.091(4) C34 0.055(2) 0.0570(19) 0.0446(17) 0.0063(14) 0.0361(16) 0.0143(15) _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 O1 1.503(3) . ? S1 C9 1.792(3) . ? S1 C7 1.806(3) . ? S2 O2 1.503(2) . ? S2 C13 1.794(3) . ? S2 C19 1.811(3) . ? S3 O3 1.492(2) . ? S3 C15 1.796(3) . ? S3 C22 1.812(3) . ? S4 O4 1.498(2) . ? S4 C3 1.800(3) . ? S4 C26 1.801(3) . ? C1 O5 1.407(4) . ? C1 H1 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? O5 C2 1.371(3) . ? C2 C3 1.378(4) . ? C2 C7 1.395(4) . ? C3 C4 1.401(4) . ? C4 C5 1.379(4) . ? C4 H4 0.9500 . ? C5 C6 1.406(4) . ? C5 C41B 1.49(2) . ? C5 C41A 1.565(19) . ? C6 C7 1.379(4) . ? C6 H6 0.9500 . ? N1 C8 1.374(3) . ? N1 C34 1.462(4) . ? N1 H1C 0.8800 . ? C8 C13 1.414(4) . ? C8 C9 1.416(4) . ? C9 C10 1.387(4) . ? C10 C11 1.369(4) . ? C10 H10 0.9500 . ? C11 C12 1.407(4) . ? C11 C45A 1.523(16) . ? C11 C45B 1.537(16) . ? C12 C13 1.376(4) . ? C12 H12 0.9500 . ? N2 C14 1.408(3) . ? N2 C27 1.481(4) . ? N2 H2 0.8800 . ? C14 C19 1.396(4) . ? C14 C15 1.404(4) . ? C15 C16 1.385(4) . ? C16 C17 1.386(4) . ? C16 H16 0.9500 . ? C17 C18 1.393(4) . ? C17 C49B 1.537(15) . ? C17 C49A 1.540(15) . ? C18 C19 1.383(4) . ? C18 H18 0.9500 . ? C20 O6 1.432(4) . ? C20 H20 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? O6 C21 1.375(3) . ? C21 C22 1.386(4) . ? C21 C26 1.392(4) . ? C22 C23 1.390(4) . ? C23 C24 1.401(4) . ? C23 H23 0.9500 . ? C24 C25 1.389(4) . ? C24 C53B 1.48(3) . ? C24 C53A 1.578(14) . ? C25 C26 1.392(4) . ? C25 H25 0.9500 . ? C27 C28 1.503(4) . ? C27 H27 0.9900 . ? C27 H27A 0.9900 . ? C28 C29 1.381(5) . ? C28 C33 1.389(4) . ? C29 C30 1.386(5) . ? C29 H29 0.9500 . ? C30 C31 1.366(6) . ? C30 H30 0.9500 . ? C31 C32 1.374(6) . ? C31 H31 0.9500 . ? C32 C33 1.385(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C35A C36A 1.3900 . ? C35A C40A 1.3900 . ? C35A C34 1.493(9) . ? C36A C37A 1.3900 . ? C36A H36A 0.9500 . ? C37A C38A 1.3900 . ? C37A H37A 0.9500 . ? C38A C39A 1.3900 . ? C38A H38A 0.9500 . ? C39A C40A 1.3900 . ? C39A H39A 0.9500 . ? C40A H40A 0.9500 . ? C35B C36B 1.3900 . ? C35B C40B 1.3900 . ? C35B C34 1.521(9) . ? C36B C37B 1.3900 . ? C36B H36B 0.9500 . ? C37B C38B 1.3900 . ? C37B H37B 0.9500 . ? C38B C39B 1.3900 . ? C38B H38B 0.9500 . ? C39B C40B 1.3900 . ? C39B H39B 0.9500 . ? C40B H40B 0.9500 . ? C41A C44A 1.529(8) . ? C41A C42A 1.533(8) . ? C41A C43A 1.551(9) . ? C42A H34J 0.9800 . ? C42A H34K 0.9800 . ? C42A H34L 0.9800 . ? C43A H43A 0.9800 . ? C43A H43B 0.9800 . ? C43A H43C 0.9800 . ? C44A H44A 0.9800 . ? C44A H44B 0.9800 . ? C44A H44C 0.9800 . ? C41B C44B 1.531(9) . ? C41B C42B 1.532(9) . ? C41B C43B 1.553(9) . ? C42B H42B 0.9800 . ? C42B H42C 0.9800 . ? C42B H42D 0.9800 . ? C43B H43D 0.9800 . ? C43B H43E 0.9800 . ? C43B H43F 0.9800 . ? C44B H44D 0.9800 . ? C44B H44E 0.9800 . ? C44B H44F 0.9800 . ? C45A C46A 1.535(8) . ? C45A C47A 1.543(8) . ? C45A C48A 1.548(8) . ? C46A H46A 0.9800 . ? C46A H46B 0.9800 . ? C46A H46C 0.9800 . ? C47A H47A 0.9800 . ? C47A H47B 0.9800 . ? C47A H47C 0.9800 . ? C48A H48A 0.9800 . ? C48A H48B 0.9800 . ? C48A H48C 0.9800 . ? C45B C46B 1.535(8) . ? C45B C47B 1.542(8) . ? C45B C48B 1.549(8) . ? C46B H46D 0.9800 . ? C46B H46E 0.9800 . ? C46B H46F 0.9800 . ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? C48B H48D 0.9800 . ? C48B H48E 0.9800 . ? C48B H48F 0.9800 . ? C49A C51A 1.507(10) . ? C49A C50A 1.532(11) . ? C49A C52A 1.552(11) . ? C50A H50A 0.9800 . ? C50A H50B 0.9800 . ? C50A H50C 0.9800 . ? C51A H34G 0.9800 . ? C51A H34H 0.9800 . ? C51A H34I 0.9800 . ? C52A H52A 0.9800 . ? C52A H52B 0.9800 . ? C52A H52C 0.9800 . ? C49B C51B 1.502(10) . ? C49B C50B 1.539(11) . ? C49B C52B 1.547(11) . ? C50B H50D 0.9800 . ? C50B H50E 0.9800 . ? C50B H50F 0.9800 . ? C51B H51B 0.9800 . ? C51B H51C 0.9800 . ? C51B H51D 0.9800 . ? C52B H52D 0.9800 . ? C52B H52E 0.9800 . ? C52B H52F 0.9800 . ? C53A C55A 1.536(7) . ? C53A C54A 1.544(7) . ? C53A C56A 1.548(7) . ? C54A H54A 0.9800 . ? C54A H54B 0.9800 . ? C54A H54C 0.9800 . ? C55A H34D 0.9800 . ? C55A H34E 0.9800 . ? C55A H34F 0.9800 . ? C56A H56A 0.9800 . ? C56A H56B 0.9800 . ? C56A H56C 0.9800 . ? C53B C55B 1.536(9) . ? C53B C54B 1.544(9) . ? C53B C56B 1.552(9) . ? C54B H54D 0.9800 . ? C54B H54E 0.9800 . ? C54B H54F 0.9800 . ? C55B H55B 0.9800 . ? C55B H55C 0.9800 . ? C55B H55D 0.9800 . ? C56B H56D 0.9800 . ? C56B H56E 0.9800 . ? C56B H56F 0.9800 . ? C1S O1S 1.402(11) . ? C1S H1S 0.9800 . ? C1S H2S 0.9800 . ? C1S H3S 0.9800 . ? O1S H4S 0.8400 . ? O1W H1W 0.85(2) . ? O1W H2W 0.86(2) . ? C34 H34 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 H34C 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 S1 C9 107.12(14) . . ? O1 S1 C7 104.61(13) . . ? C9 S1 C7 96.49(12) . . ? O2 S2 C13 108.25(12) . . ? O2 S2 C19 105.21(12) . . ? C13 S2 C19 99.62(12) . . ? O3 S3 C15 109.15(13) . . ? O3 S3 C22 105.18(13) . . ? C15 S3 C22 98.55(12) . . ? O4 S4 C3 105.75(14) . . ? O4 S4 C26 106.32(14) . . ? C3 S4 C26 97.53(13) . . ? O5 C1 H1 109.5 . . ? O5 C1 H1A 109.5 . . ? H1 C1 H1A 109.5 . . ? O5 C1 H1B 109.5 . . ? H1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 O5 C1 119.4(3) . . ? O5 C2 C3 122.3(3) . . ? O5 C2 C7 119.4(3) . . ? C3 C2 C7 118.0(2) . . ? C2 C3 C4 121.0(3) . . ? C2 C3 S4 120.9(2) . . ? C4 C3 S4 118.1(2) . . ? C5 C4 C3 121.0(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 117.8(3) . . ? C4 C5 C41B 124.5(6) . . ? C6 C5 C41B 117.7(7) . . ? C4 C5 C41A 120.7(6) . . ? C6 C5 C41A 121.4(6) . . ? C7 C6 C5 120.8(3) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C2 121.2(3) . . ? C6 C7 S1 119.4(2) . . ? C2 C7 S1 119.4(2) . . ? C8 N1 C34 124.8(2) . . ? C8 N1 H1C 117.6 . . ? C34 N1 H1C 117.6 . . ? N1 C8 C13 120.1(2) . . ? N1 C8 C9 125.4(2) . . ? C13 C8 C9 114.5(2) . . ? C10 C9 C8 121.0(2) . . ? C10 C9 S1 114.8(2) . . ? C8 C9 S1 124.1(2) . . ? C11 C10 C9 124.1(3) . . ? C11 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? C10 C11 C12 115.3(2) . . ? C10 C11 C45A 123.5(5) . . ? C12 C11 C45A 121.1(5) . . ? C10 C11 C45B 124.3(5) . . ? C12 C11 C45B 120.3(4) . . ? C13 C12 C11 121.9(3) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C13 C8 122.8(2) . . ? C12 C13 S2 113.9(2) . . ? C8 C13 S2 123.2(2) . . ? C14 N2 C27 116.0(2) . . ? C14 N2 H2 122.0 . . ? C27 N2 H2 122.0 . . ? C19 C14 C15 115.4(2) . . ? C19 C14 N2 119.7(2) . . ? C15 C14 N2 125.0(2) . . ? C16 C15 C14 121.8(2) . . ? C16 C15 S3 114.8(2) . . ? C14 C15 S3 123.4(2) . . ? C15 C16 C17 122.3(3) . . ? C15 C16 H16 118.9 . . ? C17 C16 H16 118.9 . . ? C16 C17 C18 116.3(2) . . ? C16 C17 C49B 122.0(5) . . ? C18 C17 C49B 121.6(5) . . ? C16 C17 C49A 122.7(5) . . ? C18 C17 C49A 121.0(5) . . ? C19 C18 C17 121.6(2) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C18 C19 C14 122.6(2) . . ? C18 C19 S2 118.1(2) . . ? C14 C19 S2 119.3(2) . . ? O6 C20 H20 109.5 . . ? O6 C20 H20A 109.5 . . ? H20 C20 H20A 109.5 . . ? O6 C20 H20B 109.5 . . ? H20 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 O6 C20 115.5(2) . . ? O6 C21 C22 120.4(2) . . ? O6 C21 C26 121.6(2) . . ? C22 C21 C26 118.0(3) . . ? C21 C22 C23 121.3(3) . . ? C21 C22 S3 120.5(2) . . ? C23 C22 S3 118.0(2) . . ? C22 C23 C24 120.8(3) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 117.7(3) . . ? C25 C24 C53B 118.6(9) . . ? C23 C24 C53B 123.7(9) . . ? C25 C24 C53A 123.2(5) . . ? C23 C24 C53A 118.9(5) . . ? C24 C25 C26 121.2(3) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C21 120.9(3) . . ? C25 C26 S4 120.4(2) . . ? C21 C26 S4 118.6(2) . . ? N2 C27 C28 111.1(2) . . ? N2 C27 H27 109.4 . . ? C28 C27 H27 109.4 . . ? N2 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? H27 C27 H27A 108.0 . . ? C29 C28 C33 118.3(3) . . ? C29 C28 C27 120.9(3) . . ? C33 C28 C27 120.7(3) . . ? C28 C29 C30 120.9(4) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 120.0(4) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.2(4) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 119.9(4) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 120.6(4) . . ? C32 C33 H33 119.7 . . ? C28 C33 H33 119.7 . . ? C36A C35A C40A 120.0 . . ? C36A C35A C34 112.2(8) . . ? C40A C35A C34 127.7(8) . . ? C37A C36A C35A 120.0 . . ? C37A C36A H36A 120.0 . . ? C35A C36A H36A 120.0 . . ? C36A C37A C38A 120.0 . . ? C36A C37A H37A 120.0 . . ? C38A C37A H37A 120.0 . . ? C39A C38A C37A 120.0 . . ? C39A C38A H38A 120.0 . . ? C37A C38A H38A 120.0 . . ? C40A C39A C38A 120.0 . . ? C40A C39A H39A 120.0 . . ? C38A C39A H39A 120.0 . . ? C39A C40A C35A 120.0 . . ? C39A C40A H40A 120.0 . . ? C35A C40A H40A 120.0 . . ? C36B C35B C40B 120.0 . . ? C36B C35B C34 124.9(7) . . ? C40B C35B C34 115.1(7) . . ? C37B C36B C35B 120.0 . . ? C37B C36B H36B 120.0 . . ? C35B C36B H36B 120.0 . . ? C36B C37B C38B 120.0 . . ? C36B C37B H37B 120.0 . . ? C38B C37B H37B 120.0 . . ? C39B C38B C37B 120.0 . . ? C39B C38B H38B 120.0 . . ? C37B C38B H38B 120.0 . . ? C38B C39B C40B 120.0 . . ? C38B C39B H39B 120.0 . . ? C40B C39B H39B 120.0 . . ? C39B C40B C35B 120.0 . . ? C39B C40B H40B 120.0 . . ? C35B C40B H40B 120.0 . . ? C44A C41A C42A 108.8(9) . . ? C44A C41A C43A 109.8(9) . . ? C42A C41A C43A 109.2(8) . . ? C44A C41A C5 107.2(12) . . ? C42A C41A C5 113.4(15) . . ? C43A C41A C5 108.4(12) . . ? C5 C41B C44B 111.6(12) . . ? C5 C41B C42B 109.4(16) . . ? C44B C41B C42B 108.5(9) . . ? C5 C41B C43B 109.0(13) . . ? C44B C41B C43B 109.2(9) . . ? C42B C41B C43B 109.2(8) . . ? C41B C42B H42B 109.5 . . ? C41B C42B H42C 109.5 . . ? H42B C42B H42C 109.5 . . ? C41B C42B H42D 109.5 . . ? H42B C42B H42D 109.5 . . ? H42C C42B H42D 109.5 . . ? C41B C43B H43D 109.5 . . ? C41B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C41B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C41B C44B H44D 109.5 . . ? C41B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C41B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? C11 C45A C46A 107.8(9) . . ? C11 C45A C47A 110.9(10) . . ? C46A C45A C47A 111.9(8) . . ? C11 C45A C48A 111.0(9) . . ? C46A C45A C48A 108.4(8) . . ? C47A C45A C48A 106.9(8) . . ? C46B C45B C11 107.0(9) . . ? C46B C45B C47B 111.4(8) . . ? C11 C45B C47B 111.8(9) . . ? C46B C45B C48B 109.2(8) . . ? C11 C45B C48B 109.3(9) . . ? C47B C45B C48B 108.0(8) . . ? C45B C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? C45B C46B H46F 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? C45B C47B H47D 109.5 . . ? C45B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? C45B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C45B C48B H48D 109.5 . . ? C45B C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? C45B C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? C51A C49A C50A 109.4(9) . . ? C51A C49A C17 113.0(9) . . ? C50A C49A C17 108.2(10) . . ? C51A C49A C52A 106.8(8) . . ? C50A C49A C52A 111.2(9) . . ? C17 C49A C52A 108.3(9) . . ? C51B C49B C17 110.0(10) . . ? C51B C49B C50B 105.9(8) . . ? C17 C49B C50B 109.8(9) . . ? C51B C49B C52B 109.7(9) . . ? C17 C49B C52B 110.5(10) . . ? C50B C49B C52B 110.8(9) . . ? C49B C50B H50D 109.5 . . ? C49B C50B H50E 109.5 . . ? H50D C50B H50E 109.5 . . ? C49B C50B H50F 109.5 . . ? H50D C50B H50F 109.5 . . ? H50E C50B H50F 109.5 . . ? C49B C51B H51B 109.5 . . ? C49B C51B H51C 109.5 . . ? H51B C51B H51C 109.5 . . ? C49B C51B H51D 109.5 . . ? H51B C51B H51D 109.5 . . ? H51C C51B H51D 109.5 . . ? C49B C52B H52D 109.5 . . ? C49B C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? C49B C52B H52F 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? C55A C53A C54A 110.0(7) . . ? C55A C53A C56A 109.6(6) . . ? C54A C53A C56A 107.5(6) . . ? C55A C53A C24 107.6(9) . . ? C54A C53A C24 111.6(10) . . ? C56A C53A C24 110.6(9) . . ? C24 C53B C55B 109.8(17) . . ? C24 C53B C54B 109.1(17) . . ? C55B C53B C54B 109.2(11) . . ? C24 C53B C56B 111.3(17) . . ? C55B C53B C56B 110.1(11) . . ? C54B C53B C56B 107.2(10) . . ? C53B C54B H54D 109.5 . . ? C53B C54B H54E 109.5 . . ? H54D C54B H54E 109.5 . . ? C53B C54B H54F 109.5 . . ? H54D C54B H54F 109.5 . . ? H54E C54B H54F 109.5 . . ? C53B C55B H55B 109.5 . . ? C53B C55B H55C 109.5 . . ? H55B C55B H55C 109.5 . . ? C53B C55B H55D 109.5 . . ? H55B C55B H55D 109.5 . . ? H55C C55B H55D 109.5 . . ? C53B C56B H56D 109.5 . . ? C53B C56B H56E 109.5 . . ? H56D C56B H56E 109.5 . . ? C53B C56B H56F 109.5 . . ? H56D C56B H56F 109.5 . . ? H56E C56B H56F 109.5 . . ? O1S C1S H1S 109.5 . . ? O1S C1S H2S 109.5 . . ? H1S C1S H2S 109.5 . . ? O1S C1S H3S 109.5 . . ? H1S C1S H3S 109.5 . . ? H2S C1S H3S 109.5 . . ? C1S O1S H4S 109.5 . . ? H1W O1W H2W 103(3) . . ? N1 C34 C35A 108.9(5) . . ? N1 C34 C35B 113.1(5) . . ? N1 C34 H34 109.9 . . ? C35A C34 H34 109.9 . . ? C35B C34 H34 108.6 . . ? N1 C34 H34A 109.9 . . ? C35A C34 H34A 109.9 . . ? C35B C34 H34A 106.9 . . ? H34 C34 H34A 108.3 . . ? N1 C34 H34B 109.0 . . ? C35A C34 H34B 110.2 . . ? C35B C34 H34B 109.0 . . ? H34A C34 H34B 108.9 . . ? N1 C34 H34C 109.0 . . ? C35A C34 H34C 111.9 . . ? C35B C34 H34C 109.0 . . ? H34 C34 H34C 107.2 . . ? H34B C34 H34C 107.8 . . ? 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 C1 O5 C2 C3 85.1(4) . . . . ? C1 O5 C2 C7 -100.7(4) . . . . ? O5 C2 C3 C4 171.4(3) . . . . ? C7 C2 C3 C4 -2.9(4) . . . . ? O5 C2 C3 S4 -8.9(4) . . . . ? C7 C2 C3 S4 176.8(2) . . . . ? O4 S4 C3 C2 -168.4(2) . . . . ? C26 S4 C3 C2 82.2(2) . . . . ? O4 S4 C3 C4 11.3(3) . . . . ? C26 S4 C3 C4 -98.1(2) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? S4 C3 C4 C5 -179.6(2) . . . . ? C3 C4 C5 C6 3.1(4) . . . . ? C3 C4 C5 C41B -178.5(8) . . . . ? C3 C4 C5 C41A -172.5(7) . . . . ? C4 C5 C6 C7 -3.5(4) . . . . ? C41B C5 C6 C7 178.0(8) . . . . ? C41A C5 C6 C7 172.0(7) . . . . ? C5 C6 C7 C2 0.8(4) . . . . ? C5 C6 C7 S1 -179.3(2) . . . . ? O5 C2 C7 C6 -172.0(3) . . . . ? C3 C2 C7 C6 2.4(4) . . . . ? O5 C2 C7 S1 8.0(4) . . . . ? C3 C2 C7 S1 -177.5(2) . . . . ? O1 S1 C7 C6 -4.5(3) . . . . ? C9 S1 C7 C6 105.2(2) . . . . ? O1 S1 C7 C2 175.5(2) . . . . ? C9 S1 C7 C2 -74.9(2) . . . . ? C34 N1 C8 C13 -155.0(3) . . . . ? C34 N1 C8 C9 23.8(4) . . . . ? N1 C8 C9 C10 -172.2(3) . . . . ? C13 C8 C9 C10 6.6(4) . . . . ? N1 C8 C9 S1 10.7(4) . . . . ? C13 C8 C9 S1 -170.5(2) . . . . ? O1 S1 C9 C10 49.0(2) . . . . ? C7 S1 C9 C10 -58.5(2) . . . . ? O1 S1 C9 C8 -133.7(2) . . . . ? C7 S1 C9 C8 118.8(2) . . . . ? C8 C9 C10 C11 -3.5(4) . . . . ? S1 C9 C10 C11 173.9(2) . . . . ? C9 C10 C11 C12 -1.7(4) . . . . ? C9 C10 C11 C45A -178.5(5) . . . . ? C9 C10 C11 C45B -178.4(5) . . . . ? C10 C11 C12 C13 3.4(4) . . . . ? C45A C11 C12 C13 -179.7(5) . . . . ? C45B C11 C12 C13 -179.8(5) . . . . ? C11 C12 C13 C8 0.1(4) . . . . ? C11 C12 C13 S2 176.2(2) . . . . ? N1 C8 C13 C12 173.9(2) . . . . ? C9 C8 C13 C12 -5.0(4) . . . . ? N1 C8 C13 S2 -1.9(4) . . . . ? C9 C8 C13 S2 179.21(19) . . . . ? O2 S2 C13 C12 -138.2(2) . . . . ? C19 S2 C13 C12 112.1(2) . . . . ? O2 S2 C13 C8 37.9(3) . . . . ? C19 S2 C13 C8 -71.8(2) . . . . ? C27 N2 C14 C19 -76.9(3) . . . . ? C27 N2 C14 C15 103.7(3) . . . . ? C19 C14 C15 C16 0.1(4) . . . . ? N2 C14 C15 C16 179.5(2) . . . . ? C19 C14 C15 S3 179.52(19) . . . . ? N2 C14 C15 S3 -1.1(4) . . . . ? O3 S3 C15 C16 140.6(2) . . . . ? C22 S3 C15 C16 -110.0(2) . . . . ? O3 S3 C15 C14 -38.9(3) . . . . ? C22 S3 C15 C14 70.5(2) . . . . ? C14 C15 C16 C17 -0.1(4) . . . . ? S3 C15 C16 C17 -179.6(2) . . . . ? C15 C16 C17 C18 1.1(4) . . . . ? C15 C16 C17 C49B -176.8(6) . . . . ? C15 C16 C17 C49A 179.7(6) . . . . ? C16 C17 C18 C19 -2.1(4) . . . . ? C49B C17 C18 C19 175.8(6) . . . . ? C49A C17 C18 C19 179.2(6) . . . . ? C17 C18 C19 C14 2.2(4) . . . . ? C17 C18 C19 S2 -176.0(2) . . . . ? C15 C14 C19 C18 -1.1(4) . . . . ? N2 C14 C19 C18 179.5(2) . . . . ? C15 C14 C19 S2 177.10(18) . . . . ? N2 C14 C19 S2 -2.3(3) . . . . ? O2 S2 C19 C18 -8.6(2) . . . . ? C13 S2 C19 C18 103.4(2) . . . . ? O2 S2 C19 C14 173.1(2) . . . . ? C13 S2 C19 C14 -74.9(2) . . . . ? C20 O6 C21 C22 98.8(3) . . . . ? C20 O6 C21 C26 -84.8(3) . . . . ? O6 C21 C22 C23 -179.6(2) . . . . ? C26 C21 C22 C23 3.8(4) . . . . ? O6 C21 C22 S3 -4.2(4) . . . . ? C26 C21 C22 S3 179.2(2) . . . . ? O3 S3 C22 C21 175.3(2) . . . . ? C15 S3 C22 C21 62.7(2) . . . . ? O3 S3 C22 C23 -9.1(3) . . . . ? C15 S3 C22 C23 -121.7(2) . . . . ? C21 C22 C23 C24 -2.6(4) . . . . ? S3 C22 C23 C24 -178.1(2) . . . . ? C22 C23 C24 C25 0.6(4) . . . . ? C22 C23 C24 C53B 177.6(10) . . . . ? C22 C23 C24 C53A 175.7(5) . . . . ? C23 C24 C25 C26 0.1(4) . . . . ? C53B C24 C25 C26 -177.1(10) . . . . ? C53A C24 C25 C26 -174.8(6) . . . . ? C24 C25 C26 C21 1.2(4) . . . . ? C24 C25 C26 S4 176.9(2) . . . . ? O6 C21 C26 C25 -179.7(2) . . . . ? C22 C21 C26 C25 -3.1(4) . . . . ? O6 C21 C26 S4 4.6(3) . . . . ? C22 C21 C26 S4 -178.9(2) . . . . ? O4 S4 C26 C25 -41.8(3) . . . . ? C3 S4 C26 C25 67.1(3) . . . . ? O4 S4 C26 C21 134.0(2) . . . . ? C3 S4 C26 C21 -117.1(2) . . . . ? C14 N2 C27 C28 168.5(2) . . . . ? N2 C27 C28 C29 -110.7(3) . . . . ? N2 C27 C28 C33 70.7(4) . . . . ? C33 C28 C29 C30 0.8(5) . . . . ? C27 C28 C29 C30 -177.8(3) . . . . ? C28 C29 C30 C31 -1.2(6) . . . . ? C29 C30 C31 C32 0.9(6) . . . . ? C30 C31 C32 C33 0.0(6) . . . . ? C31 C32 C33 C28 -0.4(6) . . . . ? C29 C28 C33 C32 0.1(5) . . . . ? C27 C28 C33 C32 178.7(3) . . . . ? C40A C35A C36A C37A 0.0 . . . . ? C34 C35A C36A C37A -178.4(9) . . . . ? C35A C36A C37A C38A 0.0 . . . . ? C36A C37A C38A C39A 0.0 . . . . ? C37A C38A C39A C40A 0.0 . . . . ? C38A C39A C40A C35A 0.0 . . . . ? C36A C35A C40A C39A 0.0 . . . . ? C34 C35A C40A C39A 178.1(10) . . . . ? C40B C35B C36B C37B 0.0 . . . . ? C34 C35B C36B C37B -179.8(10) . . . . ? C35B C36B C37B C38B 0.0 . . . . ? C36B C37B C38B C39B 0.0 . . . . ? C37B C38B C39B C40B 0.0 . . . . ? C38B C39B C40B C35B 0.0 . . . . ? C36B C35B C40B C39B 0.0 . . . . ? C34 C35B C40B C39B 179.8(9) . . . . ? C4 C5 C41A C44A 118.5(8) . . . . ? C6 C5 C41A C44A -56.9(11) . . . . ? C41B C5 C41A C44A -113(10) . . . . ? C4 C5 C41A C42A -1.6(11) . . . . ? C6 C5 C41A C42A -177.0(8) . . . . ? C41B C5 C41A C42A 127(10) . . . . ? C4 C5 C41A C43A -123.0(8) . . . . ? C6 C5 C41A C43A 61.6(10) . . . . ? C41B C5 C41A C43A 5(9) . . . . ? C4 C5 C41B C44B 137.0(8) . . . . ? C6 C5 C41B C44B -44.6(12) . . . . ? C41A C5 C41B C44B 82(10) . . . . ? C4 C5 C41B C42B 16.9(12) . . . . ? C6 C5 C41B C42B -164.7(9) . . . . ? C41A C5 C41B C42B -38(9) . . . . ? C4 C5 C41B C43B -102.4(9) . . . . ? C6 C5 C41B C43B 76.0(10) . . . . ? C41A C5 C41B C43B -157(10) . . . . ? C10 C11 C45A C46A 101.3(7) . . . . ? C12 C11 C45A C46A -75.3(8) . . . . ? C45B C11 C45A C46A -73(67) . . . . ? C10 C11 C45A C47A -21.5(9) . . . . ? C12 C11 C45A C47A 161.9(6) . . . . ? C45B C11 C45A C47A 164(67) . . . . ? C10 C11 C45A C48A -140.2(6) . . . . ? C12 C11 C45A C48A 43.2(9) . . . . ? C45B C11 C45A C48A 46(66) . . . . ? C10 C11 C45B C46B 123.0(6) . . . . ? C12 C11 C45B C46B -53.5(8) . . . . ? C45A C11 C45B C46B 129(67) . . . . ? C10 C11 C45B C47B 0.8(10) . . . . ? C12 C11 C45B C47B -175.8(6) . . . . ? C45A C11 C45B C47B 7(66) . . . . ? C10 C11 C45B C48B -118.8(6) . . . . ? C12 C11 C45B C48B 64.7(8) . . . . ? C45A C11 C45B C48B -113(67) . . . . ? C16 C17 C49A C51A 12.5(11) . . . . ? C18 C17 C49A C51A -169.0(6) . . . . ? C49B C17 C49A C51A -66(17) . . . . ? C16 C17 C49A C50A 133.7(7) . . . . ? C18 C17 C49A C50A -47.7(9) . . . . ? C49B C17 C49A C50A 55(17) . . . . ? C16 C17 C49A C52A -105.6(7) . . . . ? C18 C17 C49A C52A 72.9(9) . . . . ? C49B C17 C49A C52A 176(18) . . . . ? C16 C17 C49B C51B -83.7(9) . . . . ? C18 C17 C49B C51B 98.5(9) . . . . ? C49A C17 C49B C51B 20(17) . . . . ? C16 C17 C49B C50B 32.5(10) . . . . ? C18 C17 C49B C50B -145.3(6) . . . . ? C49A C17 C49B C50B 136(18) . . . . ? C16 C17 C49B C52B 155.0(6) . . . . ? C18 C17 C49B C52B -22.8(10) . . . . ? C49A C17 C49B C52B -101(18) . . . . ? C25 C24 C53A C55A 96.4(8) . . . . ? C23 C24 C53A C55A -78.5(9) . . . . ? C53B C24 C53A C55A 120(14) . . . . ? C25 C24 C53A C54A -142.9(8) . . . . ? C23 C24 C53A C54A 42.3(10) . . . . ? C53B C24 C53A C54A -119(14) . . . . ? C25 C24 C53A C56A -23.3(10) . . . . ? C23 C24 C53A C56A 161.9(8) . . . . ? C53B C24 C53A C56A 0(13) . . . . ? C25 C24 C53B C55B 83.7(15) . . . . ? C23 C24 C53B C55B -93.3(14) . . . . ? C53A C24 C53B C55B -74(14) . . . . ? C25 C24 C53B C54B -156.6(12) . . . . ? C23 C24 C53B C54B 26.3(17) . . . . ? C53A C24 C53B C54B 46(13) . . . . ? C25 C24 C53B C56B -38.5(17) . . . . ? C23 C24 C53B C56B 144.5(14) . . . . ? C53A C24 C53B C56B 164(15) . . . . ? C8 N1 C34 C35A 154.7(6) . . . . ? C8 N1 C34 C35B 155.8(6) . . . . ? C36A C35A C34 N1 129.8(4) . . . . ? C40A C35A C34 N1 -48.4(9) . . . . ? C36A C35A C34 C35B -37(13) . . . . ? C40A C35A C34 C35B 145(14) . . . . ? C36B C35B C34 N1 120.9(5) . . . . ? C40B C35B C34 N1 -59.0(7) . . . . ? C36B C35B C34 C35A 134(14) . . . . ? C40B C35B C34 C35A -45(13) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.623 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.059 _database_code_depnum_ccdc_archive 'CCDC 974898'