# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wong, Wai-Yeung Raymond' _publ_contact_author_email rwywong@hkbu.edu.hk loop_ _publ_author_name 'Feng-Rong Dai' 'Wen-Jun Wu' 'Qi-Wei Wang' 'He Tian' ; Wai-Yeung Raymond Wong ; data_L1 _database_code_depnum_ccdc_archive 'CCDC 789721' #TrackingRef '- L1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H44 N2 S2' _chemical_formula_sum 'C34 H44 N2 S2' _chemical_formula_weight 544.83 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.5379(4) _cell_length_b 14.5782(11) _cell_length_c 19.5515(14) _cell_angle_alpha 107.1120(10) _cell_angle_beta 92.4750(10) _cell_angle_gamma 91.9740(10) _cell_volume 1505.32(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9521 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 0.202 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7881 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9521 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6869 _reflns_number_gt 5758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. The low completeness of the data is due to the poor diffraction ability of the crystals. ; _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^)+(0.0984P)^2^+0.5587P] 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 6869 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1539 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 C1 C 0.0224(3) 0.97813(11) 0.46151(8) 0.0254(3) Uani 1 1 d . . . C2 C 0.2138(3) 0.92090(12) 0.44513(8) 0.0258(3) Uani 1 1 d . . . H2A H 0.3139 0.9101 0.4811 0.031 Uiso 1 1 calc R . . C3 C 0.2549(3) 0.88000(13) 0.37516(9) 0.0334(4) Uani 1 1 d . . . H3A H 0.3839 0.8401 0.3638 0.040 Uiso 1 1 calc R . . C4 C 0.1103(3) 0.89544(11) 0.31916(8) 0.0257(3) Uani 1 1 d . . . C5 C -0.0831(3) 0.95474(13) 0.33893(9) 0.0309(4) Uani 1 1 d . . . H5A H -0.1835 0.9667 0.3035 0.037 Uiso 1 1 calc R . . C6 C 0.1633(3) 0.85113(11) 0.24368(8) 0.0245(3) Uani 1 1 d . . . C7 C 0.0349(3) 0.85222(12) 0.18214(9) 0.0276(3) Uani 1 1 d . . . H7A H -0.1093 0.8832 0.1826 0.033 Uiso 1 1 calc R . . C8 C 0.1421(3) 0.80180(12) 0.11765(9) 0.0275(3) Uani 1 1 d . . . C9 C 0.3525(3) 0.76324(13) 0.13219(9) 0.0300(4) Uani 1 1 d . . . H9A H 0.4481 0.7274 0.0970 0.036 Uiso 1 1 calc R . . C10 C 0.0321(3) 0.79202(14) 0.04379(9) 0.0336(4) Uani 1 1 d . . . H10A H -0.0078 0.8553 0.0413 0.040 Uiso 1 1 calc R . . H10B H -0.1178 0.7531 0.0368 0.040 Uiso 1 1 calc R . . C11 C 0.1942(3) 0.74699(13) -0.01724(9) 0.0319(4) Uani 1 1 d . . . H11A H 0.3477 0.7837 -0.0090 0.038 Uiso 1 1 calc R . . H11B H 0.2265 0.6823 -0.0166 0.038 Uiso 1 1 calc R . . C12 C 0.0857(3) 0.74281(14) -0.09102(9) 0.0329(4) Uani 1 1 d . . . H12A H 0.0698 0.8077 -0.0937 0.039 Uiso 1 1 calc R . . H12B H -0.0750 0.7118 -0.0976 0.039 Uiso 1 1 calc R . . C13 C 0.2398(3) 0.68811(13) -0.15117(9) 0.0319(4) Uani 1 1 d . . . H13A H 0.2518 0.6229 -0.1487 0.038 Uiso 1 1 calc R . . H13B H 0.4018 0.7181 -0.1432 0.038 Uiso 1 1 calc R . . C14 C 0.1434(3) 0.68415(13) -0.22641(9) 0.0313(4) Uani 1 1 d . . . H14A H -0.0224 0.6581 -0.2336 0.038 Uiso 1 1 calc R . . H14B H 0.1426 0.7490 -0.2303 0.038 Uiso 1 1 calc R . . C15 C 0.2924(3) 0.62311(12) -0.28534(9) 0.0293(3) Uani 1 1 d . . . H15A H 0.4594 0.6478 -0.2769 0.035 Uiso 1 1 calc R . . H15B H 0.2883 0.5578 -0.2824 0.035 Uiso 1 1 calc R . . C16 C 0.2043(4) 0.62119(13) -0.36074(9) 0.0341(4) Uani 1 1 d . . . H16A H 0.0357 0.5985 -0.3688 0.041 Uiso 1 1 calc R . . H16B H 0.2144 0.6861 -0.3645 0.041 Uiso 1 1 calc R . . C17 C 0.3504(4) 0.55691(15) -0.41862(10) 0.0404(4) Uani 1 1 d . . . H17A H 0.2880 0.5581 -0.4649 0.061 Uiso 1 1 calc R . . H17B H 0.3384 0.4923 -0.4158 0.061 Uiso 1 1 calc R . . H17C H 0.5169 0.5798 -0.4116 0.061 Uiso 1 1 calc R . . C18 C 1.2184(3) 0.51657(13) 0.15047(9) 0.0324(4) Uani 1 1 d . . . H18A H 1.3471 0.4992 0.1754 0.039 Uiso 1 1 calc R . . C19 C 1.0364(3) 0.57055(11) 0.18793(8) 0.0254(3) Uani 1 1 d . . . C20 C 0.8493(3) 0.59302(13) 0.14602(9) 0.0306(4) Uani 1 1 d . . . H20A H 0.7263 0.6291 0.1698 0.037 Uiso 1 1 calc R . . C21 C 0.8338(3) 0.56665(11) 0.07461(8) 0.0229(3) Uani 1 1 d . . . H21A H 0.7045 0.5836 0.0497 0.028 Uiso 1 1 calc R . . C22 C 1.0124(3) 0.51446(12) 0.03958(8) 0.0269(3) Uani 1 1 d . . . C23 C 1.0331(3) 0.60219(12) 0.26640(8) 0.0254(3) Uani 1 1 d . . . C24 C 0.8739(3) 0.65993(12) 0.30864(9) 0.0275(3) Uani 1 1 d . . . H24A H 0.7464 0.6868 0.2901 0.033 Uiso 1 1 calc R . . C25 C 0.9205(3) 0.67529(12) 0.38362(9) 0.0262(3) Uani 1 1 d . . . C26 C 1.1175(3) 0.62785(14) 0.39648(9) 0.0323(4) Uani 1 1 d . . . H26A H 1.1759 0.6290 0.4421 0.039 Uiso 1 1 calc R . . C27 C 0.7666(3) 0.73595(12) 0.43922(9) 0.0287(3) Uani 1 1 d . . . H27A H 0.6011 0.7097 0.4293 0.034 Uiso 1 1 calc R . . H27B H 0.7686 0.8001 0.4340 0.034 Uiso 1 1 calc R . . C28 C 0.8402(3) 0.74430(13) 0.51681(9) 0.0300(4) Uani 1 1 d . . . H28A H 1.0029 0.7733 0.5281 0.036 Uiso 1 1 calc R . . H28B H 0.8420 0.6805 0.5226 0.036 Uiso 1 1 calc R . . C29 C 0.6694(3) 0.80440(13) 0.56913(9) 0.0301(4) Uani 1 1 d . . . H29A H 0.6670 0.8679 0.5628 0.036 Uiso 1 1 calc R . . H29B H 0.5070 0.7751 0.5575 0.036 Uiso 1 1 calc R . . C30 C 0.7372(3) 0.81490(12) 0.64742(9) 0.0295(3) Uani 1 1 d . . . H30A H 0.9028 0.8408 0.6585 0.035 Uiso 1 1 calc R . . H30B H 0.7296 0.7518 0.6546 0.035 Uiso 1 1 calc R . . C31 C 0.5727(3) 0.88016(13) 0.69899(9) 0.0298(3) Uani 1 1 d . . . H31A H 0.5794 0.9429 0.6913 0.036 Uiso 1 1 calc R . . H31B H 0.4074 0.8540 0.6878 0.036 Uiso 1 1 calc R . . C32 C 0.6373(4) 0.89243(13) 0.77767(9) 0.0332(4) Uani 1 1 d . . . H32A H 0.6268 0.8300 0.7859 0.040 Uiso 1 1 calc R . . H32B H 0.8035 0.9176 0.7889 0.040 Uiso 1 1 calc R . . C33 C 0.4738(4) 0.95937(14) 0.82788(10) 0.0397(4) Uani 1 1 d . . . H33A H 0.4870 1.0221 0.8202 0.048 Uiso 1 1 calc R . . H33B H 0.3074 0.9349 0.8158 0.048 Uiso 1 1 calc R . . C34 C 0.5326(6) 0.97077(19) 0.90659(12) 0.0623(7) Uani 1 1 d . . . H34A H 0.4227 1.0135 0.9352 0.094 Uiso 1 1 calc R . . H34B H 0.6955 0.9968 0.9194 0.094 Uiso 1 1 calc R . . H34C H 0.5168 0.9092 0.9149 0.094 Uiso 1 1 calc R . . N1 N -0.1282(3) 0.99579(12) 0.40953(8) 0.0357(3) Uani 1 1 d . . . N2 N 1.2076(3) 0.48891(13) 0.07641(9) 0.0419(4) Uani 1 1 d . . . S1 S 0.42092(8) 0.78802(3) 0.22219(2) 0.03018(13) Uani 1 1 d . . . S2 S 1.24581(8) 0.56558(4) 0.31866(2) 0.03515(14) 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 0.0256(7) 0.0269(7) 0.0216(8) 0.0041(6) 0.0019(6) 0.0000(6) C2 0.0283(8) 0.0320(8) 0.0161(7) 0.0049(6) 0.0015(6) 0.0078(6) C3 0.0366(9) 0.0390(9) 0.0236(8) 0.0068(7) 0.0041(7) 0.0097(7) C4 0.0276(8) 0.0268(7) 0.0209(7) 0.0042(6) 0.0028(6) -0.0003(6) C5 0.0313(9) 0.0335(8) 0.0253(8) 0.0041(6) 0.0020(6) 0.0047(7) C6 0.0236(7) 0.0269(7) 0.0220(7) 0.0054(6) 0.0027(6) 0.0026(6) C7 0.0243(8) 0.0343(8) 0.0230(8) 0.0058(6) 0.0022(6) 0.0051(6) C8 0.0279(8) 0.0317(8) 0.0210(7) 0.0050(6) 0.0028(6) 0.0008(6) C9 0.0312(8) 0.0356(9) 0.0216(7) 0.0050(6) 0.0055(6) 0.0062(7) C10 0.0324(9) 0.0453(10) 0.0207(8) 0.0057(7) 0.0016(6) 0.0052(7) C11 0.0335(9) 0.0386(9) 0.0220(8) 0.0062(7) 0.0034(6) 0.0029(7) C12 0.0365(9) 0.0389(9) 0.0212(8) 0.0055(7) 0.0019(7) 0.0033(7) C13 0.0351(9) 0.0373(9) 0.0213(8) 0.0053(7) 0.0020(6) 0.0046(7) C14 0.0366(9) 0.0338(8) 0.0215(8) 0.0043(6) 0.0027(7) 0.0068(7) C15 0.0329(8) 0.0316(8) 0.0225(8) 0.0056(6) 0.0037(6) 0.0054(7) C16 0.0445(10) 0.0351(9) 0.0229(8) 0.0076(7) 0.0037(7) 0.0082(8) C17 0.0554(12) 0.0421(10) 0.0229(8) 0.0065(7) 0.0079(8) 0.0101(9) C18 0.0284(8) 0.0414(9) 0.0256(8) 0.0065(7) 0.0013(6) 0.0081(7) C19 0.0260(8) 0.0261(7) 0.0228(7) 0.0048(6) 0.0029(6) 0.0010(6) C20 0.0299(8) 0.0371(9) 0.0226(8) 0.0044(6) 0.0029(6) 0.0087(7) C21 0.0217(7) 0.0297(7) 0.0148(7) 0.0019(5) 0.0005(5) 0.0073(6) C22 0.0269(8) 0.0287(8) 0.0220(8) 0.0029(6) 0.0026(6) -0.0003(6) C23 0.0250(7) 0.0280(7) 0.0229(8) 0.0077(6) -0.0002(6) 0.0001(6) C24 0.0306(8) 0.0302(8) 0.0212(7) 0.0064(6) 0.0002(6) 0.0043(6) C25 0.0283(8) 0.0275(7) 0.0220(8) 0.0064(6) 0.0015(6) -0.0011(6) C26 0.0303(8) 0.0450(10) 0.0209(8) 0.0087(7) 0.0003(6) 0.0050(7) C27 0.0305(8) 0.0333(8) 0.0208(7) 0.0056(6) 0.0005(6) 0.0024(7) C28 0.0319(9) 0.0361(9) 0.0207(8) 0.0060(6) 0.0016(6) 0.0042(7) C29 0.0304(8) 0.0364(9) 0.0223(8) 0.0066(6) 0.0019(6) 0.0032(7) C30 0.0312(8) 0.0329(8) 0.0230(8) 0.0051(6) 0.0027(6) 0.0052(7) C31 0.0310(8) 0.0325(8) 0.0234(8) 0.0041(6) 0.0031(6) 0.0035(7) C32 0.0403(10) 0.0330(9) 0.0242(8) 0.0051(7) 0.0027(7) 0.0032(7) C33 0.0500(12) 0.0372(9) 0.0279(9) 0.0026(7) 0.0081(8) 0.0032(8) C34 0.100(2) 0.0541(13) 0.0258(10) 0.0004(9) 0.0125(11) 0.0013(13) N1 0.0362(8) 0.0394(8) 0.0279(8) 0.0042(6) 0.0017(6) 0.0058(6) N2 0.0396(9) 0.0493(10) 0.0335(9) 0.0066(7) 0.0026(7) 0.0087(7) S1 0.0296(2) 0.0377(2) 0.0224(2) 0.00643(16) 0.00282(15) 0.01141(17) S2 0.0307(2) 0.0502(3) 0.0242(2) 0.00927(19) 0.00116(16) 0.01373(19) _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 C2 1.362(2) . ? C1 N1 1.375(2) . ? C1 C1 1.487(3) 2_576 ? C2 C3 1.355(2) . ? C2 H2A 0.9300 . ? C3 C4 1.404(2) . ? C3 H3A 0.9300 . ? C4 C5 1.395(2) . ? C4 C6 1.473(2) . ? C5 N1 1.371(2) . ? C5 H5A 0.9300 . ? C6 C7 1.375(2) . ? C6 S1 1.7245(16) . ? C7 C8 1.425(2) . ? C7 H7A 0.9300 . ? C8 C9 1.366(3) . ? C8 C10 1.508(2) . ? C9 S1 1.7115(17) . ? C9 H9A 0.9300 . ? C10 C11 1.528(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.522(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.526(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.527(2) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.526(2) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.525(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.523(2) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N2 1.382(2) . ? C18 C19 1.397(2) . ? C18 H18A 0.9300 . ? C19 C20 1.400(2) . ? C19 C23 1.467(2) . ? C20 C21 1.333(2) . ? C20 H20A 0.9300 . ? C21 C22 1.352(2) . ? C21 H21A 0.9300 . ? C22 N2 1.395(2) . ? C22 C22 1.478(3) 2_765 ? C23 C24 1.368(2) . ? C23 S2 1.7253(17) . ? C24 C25 1.427(2) . ? C24 H24A 0.9300 . ? C25 C26 1.365(3) . ? C25 C27 1.502(2) . ? C26 S2 1.7230(18) . ? C26 H26A 0.9300 . ? C27 C28 1.522(2) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.524(2) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.522(2) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.525(2) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.521(2) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.520(3) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.518(3) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 122.17(14) . . ? C2 C1 C1 117.96(19) . 2_576 ? N1 C1 C1 119.87(19) . 2_576 ? C3 C2 C1 118.44(15) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 122.62(17) . . ? C2 C3 H3A 118.7 . . ? C4 C3 H3A 118.7 . . ? C5 C4 C3 116.57(15) . . ? C5 C4 C6 122.34(15) . . ? C3 C4 C6 121.09(16) . . ? N1 C5 C4 121.41(17) . . ? N1 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? C7 C6 C4 129.52(15) . . ? C7 C6 S1 109.95(12) . . ? C4 C6 S1 120.53(12) . . ? C6 C7 C8 114.17(15) . . ? C6 C7 H7A 122.9 . . ? C8 C7 H7A 122.9 . . ? C9 C8 C7 110.97(15) . . ? C9 C8 C10 125.41(15) . . ? C7 C8 C10 123.61(16) . . ? C8 C9 S1 112.62(13) . . ? C8 C9 H9A 123.7 . . ? S1 C9 H9A 123.7 . . ? C8 C10 C11 114.51(15) . . ? C8 C10 H10A 108.6 . . ? C11 C10 H10A 108.6 . . ? C8 C10 H10B 108.6 . . ? C11 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? C12 C11 C10 113.70(15) . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? C10 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C11 C12 C13 112.27(15) . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 C14 114.57(15) . . ? C12 C13 H13A 108.6 . . ? C14 C13 H13A 108.6 . . ? C12 C13 H13B 108.6 . . ? C14 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C13 113.03(15) . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C14 113.82(15) . . ? C16 C15 H15A 108.8 . . ? C14 C15 H15A 108.8 . . ? C16 C15 H15B 108.8 . . ? C14 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C15 112.71(16) . . ? C17 C16 H16A 109.0 . . ? C15 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 C19 120.12(17) . . ? N2 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C18 C19 C20 116.02(15) . . ? C18 C19 C23 123.60(16) . . ? C20 C19 C23 120.38(15) . . ? C21 C20 C19 124.99(16) . . ? C21 C20 H20A 117.5 . . ? C19 C20 H20A 117.5 . . ? C20 C21 C22 117.86(15) . . ? C20 C21 H21A 121.1 . . ? C22 C21 H21A 121.1 . . ? C21 C22 N2 121.57(15) . . ? C21 C22 C22 116.32(19) . 2_765 ? N2 C22 C22 122.10(19) . 2_765 ? C24 C23 C19 128.60(15) . . ? C24 C23 S2 110.33(12) . . ? C19 C23 S2 121.06(13) . . ? C23 C24 C25 114.20(15) . . ? C23 C24 H24A 122.9 . . ? C25 C24 H24A 122.9 . . ? C26 C25 C24 111.15(15) . . ? C26 C25 C27 126.10(15) . . ? C24 C25 C27 122.75(15) . . ? C25 C26 S2 112.32(13) . . ? C25 C26 H26A 123.8 . . ? S2 C26 H26A 123.8 . . ? C25 C27 C28 116.04(15) . . ? C25 C27 H27A 108.3 . . ? C28 C27 H27A 108.3 . . ? C25 C27 H27B 108.3 . . ? C28 C27 H27B 108.3 . . ? H27A C27 H27B 107.4 . . ? C27 C28 C29 112.33(15) . . ? C27 C28 H28A 109.1 . . ? C29 C28 H28A 109.1 . . ? C27 C28 H28B 109.1 . . ? C29 C28 H28B 109.1 . . ? H28A C28 H28B 107.9 . . ? C30 C29 C28 114.01(15) . . ? C30 C29 H29A 108.8 . . ? C28 C29 H29A 108.8 . . ? C30 C29 H29B 108.8 . . ? C28 C29 H29B 108.8 . . ? H29A C29 H29B 107.6 . . ? C29 C30 C31 113.06(15) . . ? C29 C30 H30A 109.0 . . ? C31 C30 H30A 109.0 . . ? C29 C30 H30B 109.0 . . ? C31 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? C32 C31 C30 114.18(15) . . ? C32 C31 H31A 108.7 . . ? C30 C31 H31A 108.7 . . ? C32 C31 H31B 108.7 . . ? C30 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C33 C32 C31 113.06(16) . . ? C33 C32 H32A 109.0 . . ? C31 C32 H32A 109.0 . . ? C33 C32 H32B 109.0 . . ? C31 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C34 C33 C32 113.7(2) . . ? C34 C33 H33A 108.8 . . ? C32 C33 H33A 108.8 . . ? C34 C33 H33B 108.8 . . ? C32 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C5 N1 C1 118.78(16) . . ? C18 N2 C22 119.43(16) . . ? C9 S1 C6 92.27(8) . . ? C26 S2 C23 91.99(8) . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.576 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.092 # Attachment '- L2.cif' data_L2 _database_code_depnum_ccdc_archive 'CCDC 789722' #TrackingRef '- L2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H34 N4' _chemical_formula_sum 'C46 H34 N4' _chemical_formula_weight 642.77 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.9729(15) _cell_length_b 25.621(3) _cell_length_c 11.2567(11) _cell_angle_alpha 90.00 _cell_angle_beta 128.422(2) _cell_angle_gamma 90.00 _cell_volume 3383.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3138 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 28.11 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6511 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart 1000 CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10474 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4042 _reflns_number_gt 2535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The low completeness of the data is due to the poor diffraction ability of the crystals. ; _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^)+(0.1049P)^2^+0.7853P] 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 4042 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1888 _refine_ls_wR_factor_gt 0.1609 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 N1 N 1.0000 -0.23703(8) 0.2500 0.0491(6) Uani 1 2 d S . . N2 N 1.06947(16) 0.06726(6) 0.38508(19) 0.0453(4) Uani 0.50 1 d P . . N3 N 1.07280(15) 0.17681(6) 0.3835(2) 0.0438(4) Uani 0.50 1 d P . . N4 N 1.0000 0.48150(7) 0.2500 0.0438(5) Uani 1 2 d S . . C1 C 0.92280(18) -0.26381(7) 0.2610(2) 0.0457(5) Uani 1 1 d . . . C2 C 0.9540(2) -0.31030(7) 0.3418(3) 0.0610(6) Uani 1 1 d . . . H2A H 1.0270 -0.3237 0.3921 0.073 Uiso 1 1 calc R . . C3 C 0.8751(4) -0.33649(8) 0.3467(4) 0.0866(11) Uani 1 1 d . . . H3A H 0.8957 -0.3679 0.3994 0.104 Uiso 1 1 calc R . . C4 C 0.7674(3) -0.31706(12) 0.2756(4) 0.0858(10) Uani 1 1 d . . . H4A H 0.7153 -0.3354 0.2788 0.103 Uiso 1 1 calc R . . C5 C 0.7366(2) -0.26978(11) 0.1985(3) 0.0715(7) Uani 1 1 d . . . H5A H 0.6645 -0.2558 0.1523 0.086 Uiso 1 1 calc R . . C6 C 0.81425(19) -0.24366(9) 0.1913(3) 0.0564(6) Uani 1 1 d . . . H6A H 0.7935 -0.2122 0.1392 0.068 Uiso 1 1 calc R . . C7 C 1.0000 -0.18148(9) 0.2500 0.0401(6) Uani 1 2 d S . . C8 C 0.99034(17) -0.15421(6) 0.1359(2) 0.0422(5) Uani 1 1 d . . . H8A H 0.9843 -0.1723 0.0596 0.051 Uiso 1 1 calc R . . C9 C 0.98962(16) -0.10001(6) 0.1357(2) 0.0398(4) Uani 1 1 d . . . H9A H 0.9821 -0.0820 0.0582 0.048 Uiso 1 1 calc R . . C10 C 1.0000 -0.07227(9) 0.2500 0.0358(5) Uani 1 2 d S . . C11 C 1.0000 -0.01421(9) 0.2500 0.0365(5) Uani 1 2 d S . . C12 C 1.06898(18) 0.01424(7) 0.3833(2) 0.0464(5) Uani 1 1 d . . . H12A H 1.1166 -0.0036 0.4748 0.056 Uiso 1 1 calc R . . C13 C 1.06947(16) 0.06726(6) 0.38508(19) 0.0453(4) Uani 0.50 1 d P . . H13A H 1.1160 0.0855 0.4760 0.054 Uiso 0.50 1 calc PR . . C14 C 1.0000 0.09314(9) 0.2500 0.0358(5) Uani 1 2 d S . . C15 C 1.0000 0.15102(9) 0.2500 0.0379(6) Uani 1 2 d S . . C16 C 1.07280(15) 0.17681(6) 0.3835(2) 0.0438(4) Uani 0.50 1 d P . . H16A H 1.1217 0.1584 0.4737 0.053 Uiso 0.50 1 calc PR . . C17 C 1.07312(18) 0.22989(7) 0.3834(2) 0.0456(5) Uani 1 1 d . . . H17A H 1.1234 0.2476 0.4745 0.055 Uiso 1 1 calc R . . C18 C 1.0000 0.25846(9) 0.2500 0.0399(6) Uani 1 2 d S . . C19 C 1.0000 0.31631(9) 0.2500 0.0381(6) Uani 1 2 d S . . C20 C 1.10186(16) 0.34428(6) 0.3315(2) 0.0416(4) Uani 1 1 d . . . H20A H 1.1708 0.3264 0.3871 0.050 Uiso 1 1 calc R . . C21 C 1.10197(16) 0.39838(7) 0.3310(2) 0.0413(4) Uani 1 1 d . . . H21A H 1.1709 0.4163 0.3853 0.050 Uiso 1 1 calc R . . C22 C 1.0000 0.42616(9) 0.2500 0.0389(6) Uani 1 2 d S . . C23 C 0.91845(17) 0.50945(7) 0.1141(2) 0.0427(5) Uani 1 1 d . . . C24 C 0.88417(18) 0.49103(8) -0.0239(2) 0.0507(5) Uani 1 1 d . . . H24A H 0.9120 0.4593 -0.0287 0.061 Uiso 1 1 calc R . . C25 C 0.80841(19) 0.51958(10) -0.1556(3) 0.0617(6) Uani 1 1 d . . . H25A H 0.7844 0.5066 -0.2484 0.074 Uiso 1 1 calc R . . C26 C 0.7687(2) 0.56745(10) -0.1483(3) 0.0690(7) Uani 1 1 d . . . H26A H 0.7213 0.5876 -0.2352 0.083 Uiso 1 1 calc R . . C27 C 0.79982(19) 0.58485(8) -0.0119(3) 0.0609(7) Uani 1 1 d . . . H27A H 0.7706 0.6162 -0.0077 0.073 Uiso 1 1 calc R . . C28 C 0.87360(18) 0.55644(7) 0.1184(3) 0.0490(5) Uani 1 1 d . . . H28A H 0.8937 0.5686 0.2099 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0614(15) 0.0253(10) 0.0749(17) 0.000 0.0494(14) 0.000 N2 0.0553(11) 0.0301(8) 0.0361(9) -0.0022(7) 0.0213(9) 0.0031(7) N3 0.0493(10) 0.0298(8) 0.0469(10) 0.0012(7) 0.0273(9) 0.0032(7) N4 0.0527(14) 0.0244(10) 0.0389(12) 0.000 0.0208(11) 0.000 C1 0.0617(13) 0.0326(9) 0.0514(12) -0.0068(8) 0.0394(11) -0.0091(8) C2 0.1066(19) 0.0299(9) 0.0772(16) 0.0007(10) 0.0723(16) 0.0036(11) C3 0.184(4) 0.0328(11) 0.116(2) -0.0132(13) 0.130(3) -0.0195(16) C4 0.130(3) 0.0788(18) 0.102(2) -0.0466(17) 0.099(2) -0.0594(19) C5 0.0624(15) 0.100(2) 0.0556(15) -0.0249(14) 0.0383(13) -0.0362(14) C6 0.0541(13) 0.0646(13) 0.0495(13) -0.0028(10) 0.0316(11) -0.0132(11) C7 0.0430(14) 0.0261(11) 0.0549(17) 0.000 0.0322(14) 0.000 C8 0.0521(12) 0.0333(9) 0.0493(11) -0.0067(8) 0.0356(10) -0.0057(8) C9 0.0481(11) 0.0316(8) 0.0433(11) -0.0002(7) 0.0302(9) -0.0035(7) C10 0.0369(13) 0.0278(11) 0.0408(14) 0.000 0.0232(12) 0.000 C11 0.0417(14) 0.0276(11) 0.0398(14) 0.000 0.0252(12) 0.000 C12 0.0556(12) 0.0302(9) 0.0397(11) 0.0017(7) 0.0228(10) 0.0047(8) C13 0.0553(11) 0.0301(8) 0.0361(9) -0.0022(7) 0.0213(9) 0.0031(7) C14 0.0429(11) 0.0280(11) 0.0376(14) 0.000 0.0255(11) 0.000 C15 0.0439(15) 0.0275(11) 0.0464(15) 0.000 0.0300(13) 0.000 C16 0.0493(10) 0.0298(8) 0.0469(10) 0.0012(7) 0.0273(9) 0.0032(7) C17 0.0523(12) 0.0314(9) 0.0533(12) 0.0014(8) 0.0329(11) 0.0014(8) C18 0.0455(15) 0.0270(11) 0.0523(16) 0.000 0.0329(14) 0.000 C19 0.0474(15) 0.0258(11) 0.0442(15) 0.000 0.0300(13) 0.000 C20 0.0397(10) 0.0333(9) 0.0461(11) 0.0060(7) 0.0238(9) 0.0047(7) C21 0.0414(10) 0.0310(8) 0.0462(11) 0.0009(7) 0.0245(9) -0.0024(7) C22 0.0473(15) 0.0292(11) 0.0359(14) 0.000 0.0238(13) 0.000 C23 0.0450(11) 0.0333(9) 0.0436(11) 0.0058(8) 0.0245(9) 0.0011(8) C24 0.0524(12) 0.0478(11) 0.0457(12) 0.0051(9) 0.0274(10) 0.0062(9) C25 0.0514(13) 0.0825(16) 0.0419(12) 0.0138(11) 0.0244(11) 0.0061(12) C26 0.0494(13) 0.0783(16) 0.0736(18) 0.0410(14) 0.0354(13) 0.0216(12) C27 0.0524(13) 0.0455(11) 0.0881(19) 0.0242(11) 0.0454(14) 0.0125(9) C28 0.0546(12) 0.0332(9) 0.0628(14) 0.0050(9) 0.0382(11) 0.0033(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.414(2) . ? N1 C1 1.414(2) 2_755 ? N1 C7 1.423(3) . ? N2 C14 1.367(2) . ? N3 C15 1.359(2) . ? N4 C22 1.418(3) . ? N4 C23 1.422(2) 2_755 ? N4 C23 1.422(2) . ? C1 C2 1.392(3) . ? C1 C6 1.393(3) . ? C2 C3 1.389(4) . ? C2 H2A 0.9300 . ? C3 C4 1.373(5) . ? C3 H3A 0.9300 . ? C4 C5 1.391(4) . ? C4 H4A 0.9300 . ? C5 C6 1.387(3) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.388(2) 2_755 ? C7 C8 1.388(2) . ? C8 C9 1.389(2) . ? C8 H8A 0.9300 . ? C9 C10 1.391(2) . ? C9 H9A 0.9300 . ? C10 C9 1.391(2) 2_755 ? C10 C11 1.488(3) . ? C11 C12 1.387(2) . ? C11 C12 1.387(2) 2_755 ? C12 H12A 0.9300 . ? C14 C13 1.367(2) 2_755 ? C14 N2 1.367(2) 2_755 ? C14 C15 1.483(3) . ? C15 C16 1.359(2) 2_755 ? C15 N3 1.359(2) 2_755 ? C17 C18 1.395(2) . ? C17 H17A 0.9300 . ? C18 C17 1.395(2) 2_755 ? C18 C19 1.482(3) . ? C19 C20 1.394(2) . ? C19 C20 1.394(2) 2_755 ? C20 C21 1.386(2) . ? C20 H20A 0.9300 . ? C21 C22 1.392(2) . ? C21 H21A 0.9300 . ? C22 C21 1.392(2) 2_755 ? C23 C24 1.381(3) . ? C23 C28 1.394(2) . ? C24 C25 1.389(3) . ? C24 H24A 0.9300 . ? C25 C26 1.388(3) . ? C25 H25A 0.9300 . ? C26 C27 1.372(4) . ? C26 H26A 0.9300 . ? C27 C28 1.374(3) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C1 121.9(2) . 2_755 ? C1 N1 C7 119.03(10) . . ? C1 N1 C7 119.03(10) 2_755 . ? C22 N4 C23 120.24(10) . 2_755 ? C22 N4 C23 120.24(10) . . ? C23 N4 C23 119.5(2) 2_755 . ? C2 C1 C6 119.0(2) . . ? C2 C1 N1 120.81(19) . . ? C6 C1 N1 120.16(17) . . ? C3 C2 C1 119.4(3) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C4 C3 C2 121.4(2) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 119.6(2) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C6 C5 C4 119.4(3) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C1 121.1(2) . . ? C5 C6 H6A 119.5 . . ? C1 C6 H6A 119.5 . . ? C8 C7 C8 119.6(2) 2_755 . ? C8 C7 N1 120.22(11) 2_755 . ? C8 C7 N1 120.22(11) . . ? C9 C8 C7 120.08(17) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 120.85(17) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C9 C10 C9 118.6(2) . 2_755 ? C9 C10 C11 120.72(11) . . ? C9 C10 C11 120.72(11) 2_755 . ? C12 C11 C12 116.6(2) . 2_755 ? C12 C11 C10 121.70(11) . . ? C12 C11 C10 121.70(11) 2_755 . ? C11 C12 H12A 118.8 . . ? C13 C14 N2 0.0(2) 2_755 2_755 ? C13 C14 N2 121.9(2) 2_755 . ? N2 C14 N2 121.9(2) 2_755 . ? C13 C14 C15 119.03(10) 2_755 . ? N2 C14 C15 119.03(10) 2_755 . ? N2 C14 C15 119.03(10) . . ? N3 C15 C16 121.8(2) . 2_755 ? N3 C15 N3 121.8(2) . 2_755 ? C16 C15 N3 0.0(2) 2_755 2_755 ? N3 C15 C14 119.08(11) . . ? C16 C15 C14 119.08(11) 2_755 . ? N3 C15 C14 119.08(11) 2_755 . ? C18 C17 H17A 119.2 . . ? C17 C18 C17 116.7(2) 2_755 . ? C17 C18 C19 121.66(11) 2_755 . ? C17 C18 C19 121.66(11) . . ? C20 C19 C20 118.1(2) . 2_755 ? C20 C19 C18 120.95(11) . . ? C20 C19 C18 120.95(11) 2_755 . ? C21 C20 C19 121.01(17) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C20 C21 C22 120.68(18) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C21 C22 C21 118.5(2) 2_755 . ? C21 C22 N4 120.74(11) 2_755 . ? C21 C22 N4 120.74(11) . . ? C24 C23 C28 118.93(18) . . ? C24 C23 N4 120.55(16) . . ? C28 C23 N4 120.51(18) . . ? C23 C24 C25 120.4(2) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C26 C25 C24 119.9(2) . . ? C26 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? C27 C26 C25 119.5(2) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 120.7(2) . . ? C26 C27 H27A 119.6 . . ? C28 C27 H27A 119.6 . . ? C27 C28 C23 120.4(2) . . ? C27 C28 H28A 119.8 . . ? C23 C28 H28A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.341 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.049 # Attachment '- L3.cif' data_L3 _database_code_depnum_ccdc_archive 'CCDC 789723' #TrackingRef '- L3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H38 N4 S2' _chemical_formula_sum 'C54 H38 N4 S2' _chemical_formula_weight 807.00 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7447(10) _cell_length_b 11.8346(11) _cell_length_c 17.2692(16) _cell_angle_alpha 95.596(2) _cell_angle_beta 97.058(2) _cell_angle_gamma 108.418(2) _cell_volume 2045.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12904 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.26 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7513 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12904 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.26 _reflns_number_total 9318 _reflns_number_gt 6845 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The low completeness of the data is due to the poor diffraction ability of the crystals. ; _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^)+(0.0696P)^2^+0.2196P] 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 9318 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 C1 C 1.11344(18) -0.21390(14) 0.95849(9) 0.0310(4) Uani 1 1 d . . . C2 C 1.01569(19) -0.16747(14) 0.97822(10) 0.0346(4) Uani 1 1 d . . . H2A H 0.9460 -0.1698 0.9397 0.042 Uiso 1 1 calc R . . C3 C 1.0222(2) -0.11758(16) 1.05552(11) 0.0410(4) Uani 1 1 d . . . H3A H 0.9571 -0.0859 1.0683 0.049 Uiso 1 1 calc R . . C4 C 1.1244(2) -0.11472(16) 1.11358(11) 0.0444(5) Uani 1 1 d . . . H4A H 1.1278 -0.0821 1.1653 0.053 Uiso 1 1 calc R . . C5 C 1.2217(2) -0.16083(17) 1.09392(11) 0.0444(5) Uani 1 1 d . . . H5A H 1.2905 -0.1594 1.1328 0.053 Uiso 1 1 calc R . . C6 C 1.21764(19) -0.20928(16) 1.01643(10) 0.0374(4) Uani 1 1 d . . . H6A H 1.2844 -0.2385 1.0035 0.045 Uiso 1 1 calc R . . C7 C 1.12376(17) -0.37857(14) 0.86263(10) 0.0295(3) Uani 1 1 d . . . C8 C 1.10226(18) -0.45967(15) 0.91682(10) 0.0353(4) Uani 1 1 d . . . H8A H 1.0747 -0.4397 0.9637 0.042 Uiso 1 1 calc R . . C9 C 1.1213(2) -0.56917(17) 0.90203(12) 0.0452(5) Uani 1 1 d . . . H9A H 1.1068 -0.6221 0.9390 0.054 Uiso 1 1 calc R . . C10 C 1.1619(2) -0.60090(18) 0.83246(13) 0.0533(6) Uani 1 1 d . . . H10A H 1.1748 -0.6747 0.8226 0.064 Uiso 1 1 calc R . . C11 C 1.1829(2) -0.52150(18) 0.77790(12) 0.0495(5) Uani 1 1 d . . . H11A H 1.2091 -0.5426 0.7308 0.059 Uiso 1 1 calc R . . C12 C 1.1654(2) -0.41123(16) 0.79264(11) 0.0381(4) Uani 1 1 d . . . H12A H 1.1814 -0.3582 0.7558 0.046 Uiso 1 1 calc R . . C13 C 1.07039(17) -0.20399(14) 0.81766(9) 0.0290(3) Uani 1 1 d . . . C14 C 0.98430(18) -0.26350(15) 0.74799(10) 0.0345(4) Uani 1 1 d . . . H14A H 0.9490 -0.3471 0.7398 0.041 Uiso 1 1 calc R . . C15 C 0.95123(18) -0.19861(16) 0.69112(10) 0.0348(4) Uani 1 1 d . . . H15A H 0.8947 -0.2399 0.6448 0.042 Uiso 1 1 calc R . . C16 C 1.00021(16) -0.07289(15) 0.70126(9) 0.0293(3) Uani 1 1 d . . . C17 C 1.08664(16) -0.01444(14) 0.77086(9) 0.0294(3) Uani 1 1 d . . . H17A H 1.1220 0.0691 0.7790 0.035 Uiso 1 1 calc R . . C18 C 1.12077(16) -0.07827(14) 0.82796(9) 0.0295(3) Uani 1 1 d . . . H18A H 1.1782 -0.0369 0.8740 0.035 Uiso 1 1 calc R . . C19 C 0.95861(17) -0.00617(15) 0.64136(10) 0.0309(4) Uani 1 1 d . . . C20 C 0.89414(18) -0.04843(17) 0.56567(10) 0.0361(4) Uani 1 1 d . . . H20A H 0.8713 -0.1283 0.5430 0.043 Uiso 1 1 calc R . . C21 C 0.86566(19) 0.04090(18) 0.52534(10) 0.0388(4) Uani 1 1 d . . . H21A H 0.8221 0.0254 0.4735 0.047 Uiso 1 1 calc R . . C22 C 0.90796(18) 0.15214(17) 0.56955(10) 0.0356(4) Uani 1 1 d . . . C23 C 0.8702(2) 0.34888(18) 0.60226(11) 0.0441(5) Uani 1 1 d . . . H23A H 0.8914 0.3436 0.6554 0.053 Uiso 1 1 calc R . . C24 C 0.88349(19) 0.26068(17) 0.54722(10) 0.0380(4) Uani 1 1 d . . . C25 C 0.8614(2) 0.2759(2) 0.46815(11) 0.0492(5) Uani 1 1 d . . . H25A H 0.8730 0.2223 0.4289 0.059 Uiso 1 1 calc R . . C26 C 0.8221(2) 0.3711(2) 0.44861(11) 0.0492(5) Uani 1 1 d . . . H26A H 0.8083 0.3826 0.3962 0.059 Uiso 1 1 calc R . . C27 C 0.80336(19) 0.44957(17) 0.50756(10) 0.0386(4) Uani 1 1 d . . . C28 C 0.74471(18) 0.54304(16) 0.48870(10) 0.0360(4) Uani 1 1 d . . . C29 C 0.68159(19) 0.59167(16) 0.54248(10) 0.0363(4) Uani 1 1 d . . . H29A H 0.6798 0.5687 0.5924 0.044 Uiso 1 1 calc R . . C30 C 0.62217(19) 0.67354(15) 0.52119(10) 0.0370(4) Uani 1 1 d . . . H30A H 0.5782 0.7049 0.5563 0.044 Uiso 1 1 calc R . . C31 C 0.62796(18) 0.70987(15) 0.44638(10) 0.0323(4) Uani 1 1 d . . . C32 C 0.6942(2) 0.65675(18) 0.39742(11) 0.0410(4) Uani 1 1 d . . . H32A H 0.6992 0.6796 0.3476 0.049 Uiso 1 1 calc R . . C33 C 0.56635(17) 0.79629(15) 0.42097(9) 0.0316(4) Uani 1 1 d . . . C34 C 0.4696(2) 0.82976(18) 0.45113(12) 0.0452(5) Uani 1 1 d . . . H34A H 0.4321 0.7986 0.4935 0.054 Uiso 1 1 calc R . . C35 C 0.4318(2) 0.91554(19) 0.41227(12) 0.0478(5) Uani 1 1 d . . . H35A H 0.3668 0.9462 0.4266 0.057 Uiso 1 1 calc R . . C36 C 0.49893(17) 0.95002(15) 0.35172(10) 0.0320(4) Uani 1 1 d . . . C37 C 0.48546(17) 1.03724(14) 0.29913(10) 0.0308(4) Uani 1 1 d . . . C38 C 0.57573(18) 1.07746(15) 0.24785(10) 0.0332(4) Uani 1 1 d . . . H38A H 0.6478 1.0500 0.2476 0.040 Uiso 1 1 calc R . . C39 C 0.55963(18) 1.15761(15) 0.19736(10) 0.0349(4) Uani 1 1 d . . . H39A H 0.6209 1.1831 0.1637 0.042 Uiso 1 1 calc R . . C40 C 0.45339(19) 1.20038(15) 0.19625(10) 0.0335(4) Uani 1 1 d . . . C41 C 0.3631(2) 1.16235(16) 0.24804(11) 0.0384(4) Uani 1 1 d . . . H41A H 0.2919 1.1909 0.2486 0.046 Uiso 1 1 calc R . . C42 C 0.37949(19) 1.08252(16) 0.29839(11) 0.0366(4) Uani 1 1 d . . . H42A H 0.3189 1.0582 0.3326 0.044 Uiso 1 1 calc R . . C43 C 0.44604(19) 1.25174(15) 0.06206(10) 0.0350(4) Uani 1 1 d . . . C44 C 0.41124(19) 1.13273(15) 0.02642(10) 0.0368(4) Uani 1 1 d . . . H44A H 0.3814 1.0701 0.0554 0.044 Uiso 1 1 calc R . . C45 C 0.42116(19) 1.10777(17) -0.05221(11) 0.0415(4) Uani 1 1 d . . . H45A H 0.4021 1.0284 -0.0749 0.050 Uiso 1 1 calc R . . C46 C 0.4589(2) 1.19898(19) -0.09741(11) 0.0451(5) Uani 1 1 d . . . H46A H 0.4613 1.1813 -0.1508 0.054 Uiso 1 1 calc R . . C47 C 0.4931(2) 1.31685(18) -0.06225(12) 0.0473(5) Uani 1 1 d . . . H47A H 0.5181 1.3788 -0.0924 0.057 Uiso 1 1 calc R . . C48 C 0.4908(2) 1.34407(16) 0.01743(11) 0.0421(4) Uani 1 1 d . . . H48A H 0.5190 1.4239 0.0411 0.050 Uiso 1 1 calc R . . C49 C 0.38408(17) 1.37258(14) 0.16562(10) 0.0314(4) Uani 1 1 d . . . C50 C 0.28607(18) 1.39502(17) 0.11549(11) 0.0406(4) Uani 1 1 d . . . H50A H 0.2526 1.3485 0.0662 0.049 Uiso 1 1 calc R . . C51 C 0.2380(2) 1.4863(2) 0.13847(13) 0.0510(5) Uani 1 1 d . . . H51A H 0.1736 1.5015 0.1040 0.061 Uiso 1 1 calc R . . C52 C 0.2839(2) 1.55493(19) 0.21170(13) 0.0508(5) Uani 1 1 d . . . H52A H 0.2500 1.6153 0.2271 0.061 Uiso 1 1 calc R . . C53 C 0.3815(2) 1.53269(17) 0.26206(12) 0.0448(5) Uani 1 1 d . . . H53A H 0.4134 1.5787 0.3116 0.054 Uiso 1 1 calc R . . C54 C 0.43216(19) 1.44283(16) 0.23944(11) 0.0379(4) Uani 1 1 d . . . H54A H 0.4983 1.4293 0.2735 0.045 Uiso 1 1 calc R . . N1 N 1.10601(15) -0.26539(12) 0.87863(8) 0.0329(3) Uani 1 1 d . . . N2 N 0.82969(17) 0.44004(15) 0.58460(9) 0.0433(4) Uani 1 1 d . . . N3 N 0.75081(18) 0.57601(16) 0.41640(9) 0.0451(4) Uani 1 1 d . . . N4 N 0.43503(17) 1.27921(13) 0.14259(8) 0.0384(4) Uani 1 1 d . . . S1 S 0.61061(5) 0.87306(4) 0.34244(2) 0.03510(12) Uani 1 1 d . . . S2 S 0.98357(5) 0.14671(4) 0.66294(3) 0.03800(12) 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 0.0441(10) 0.0238(8) 0.0263(8) 0.0063(6) 0.0099(7) 0.0106(7) C2 0.0458(11) 0.0296(8) 0.0328(9) 0.0100(7) 0.0115(8) 0.0150(8) C3 0.0611(13) 0.0312(9) 0.0387(10) 0.0096(7) 0.0224(9) 0.0199(9) C4 0.0633(13) 0.0355(10) 0.0298(9) 0.0014(7) 0.0142(9) 0.0088(9) C5 0.0526(12) 0.0440(11) 0.0301(9) 0.0059(8) 0.0018(8) 0.0088(9) C6 0.0418(10) 0.0358(9) 0.0343(9) 0.0058(7) 0.0074(8) 0.0117(8) C7 0.0314(9) 0.0257(8) 0.0315(8) 0.0034(6) 0.0053(7) 0.0100(7) C8 0.0419(10) 0.0307(8) 0.0327(9) 0.0060(7) 0.0068(7) 0.0105(8) C9 0.0591(13) 0.0310(9) 0.0443(11) 0.0116(8) 0.0015(9) 0.0138(9) C10 0.0769(16) 0.0330(10) 0.0551(13) 0.0001(9) 0.0053(11) 0.0294(11) C11 0.0658(14) 0.0443(11) 0.0452(11) -0.0002(9) 0.0153(10) 0.0272(10) C12 0.0487(11) 0.0348(9) 0.0343(9) 0.0059(7) 0.0127(8) 0.0163(8) C13 0.0338(9) 0.0313(8) 0.0262(8) 0.0076(6) 0.0093(7) 0.0141(7) C14 0.0396(10) 0.0287(8) 0.0334(9) 0.0045(7) 0.0065(7) 0.0086(7) C15 0.0347(9) 0.0371(9) 0.0293(9) 0.0031(7) 0.0012(7) 0.0094(8) C16 0.0293(8) 0.0352(9) 0.0266(8) 0.0079(6) 0.0085(6) 0.0128(7) C17 0.0303(9) 0.0261(8) 0.0321(8) 0.0073(6) 0.0073(7) 0.0080(7) C18 0.0299(9) 0.0316(8) 0.0268(8) 0.0035(6) 0.0037(6) 0.0103(7) C19 0.0282(9) 0.0365(9) 0.0310(8) 0.0100(7) 0.0083(7) 0.0121(7) C20 0.0371(10) 0.0428(10) 0.0293(9) 0.0052(7) 0.0053(7) 0.0144(8) C21 0.0388(10) 0.0550(11) 0.0262(9) 0.0088(8) 0.0046(7) 0.0201(9) C22 0.0356(10) 0.0493(11) 0.0288(9) 0.0146(8) 0.0079(7) 0.0198(8) C23 0.0566(13) 0.0502(11) 0.0293(9) 0.0118(8) 0.0006(8) 0.0235(10) C24 0.0384(10) 0.0507(11) 0.0330(9) 0.0170(8) 0.0085(7) 0.0221(9) C25 0.0672(14) 0.0676(14) 0.0320(10) 0.0185(9) 0.0188(9) 0.0420(12) C26 0.0676(14) 0.0715(14) 0.0298(10) 0.0245(9) 0.0183(9) 0.0437(12) C27 0.0420(11) 0.0461(10) 0.0327(9) 0.0158(8) 0.0065(8) 0.0184(9) C28 0.0377(10) 0.0419(10) 0.0306(9) 0.0138(7) 0.0042(7) 0.0143(8) C29 0.0470(11) 0.0356(9) 0.0246(8) 0.0094(7) 0.0057(7) 0.0101(8) C30 0.0469(11) 0.0338(9) 0.0287(9) 0.0054(7) 0.0081(8) 0.0104(8) C31 0.0360(9) 0.0324(8) 0.0263(8) 0.0073(6) 0.0023(7) 0.0083(7) C32 0.0509(12) 0.0535(11) 0.0302(9) 0.0196(8) 0.0119(8) 0.0278(10) C33 0.0364(9) 0.0310(8) 0.0263(8) 0.0075(6) 0.0050(7) 0.0086(7) C34 0.0503(12) 0.0502(11) 0.0477(11) 0.0267(9) 0.0244(9) 0.0224(10) C35 0.0521(12) 0.0533(12) 0.0555(12) 0.0267(10) 0.0292(10) 0.0284(10) C36 0.0350(9) 0.0309(8) 0.0326(9) 0.0091(7) 0.0090(7) 0.0117(7) C37 0.0350(9) 0.0291(8) 0.0296(8) 0.0070(6) 0.0077(7) 0.0106(7) C38 0.0350(9) 0.0337(9) 0.0350(9) 0.0084(7) 0.0114(7) 0.0141(7) C39 0.0406(10) 0.0337(9) 0.0330(9) 0.0098(7) 0.0140(7) 0.0116(8) C40 0.0450(10) 0.0274(8) 0.0305(9) 0.0074(7) 0.0095(7) 0.0130(7) C41 0.0444(11) 0.0382(10) 0.0413(10) 0.0128(8) 0.0157(8) 0.0206(8) C42 0.0409(10) 0.0368(9) 0.0391(10) 0.0138(7) 0.0186(8) 0.0155(8) C43 0.0455(11) 0.0307(8) 0.0302(9) 0.0068(7) 0.0096(7) 0.0127(8) C44 0.0424(10) 0.0289(8) 0.0362(9) 0.0054(7) 0.0067(8) 0.0076(8) C45 0.0412(11) 0.0377(10) 0.0399(10) -0.0058(8) 0.0004(8) 0.0108(8) C46 0.0498(12) 0.0579(12) 0.0305(9) 0.0028(8) 0.0077(8) 0.0227(10) C47 0.0630(14) 0.0476(11) 0.0408(11) 0.0191(9) 0.0202(10) 0.0234(10) C48 0.0604(13) 0.0301(9) 0.0403(10) 0.0106(7) 0.0174(9) 0.0164(9) C49 0.0354(9) 0.0264(8) 0.0318(9) 0.0067(6) 0.0068(7) 0.0084(7) C50 0.0337(10) 0.0458(10) 0.0386(10) 0.0072(8) 0.0032(8) 0.0085(8) C51 0.0404(11) 0.0705(14) 0.0573(13) 0.0264(11) 0.0161(10) 0.0316(11) C52 0.0613(14) 0.0482(11) 0.0617(14) 0.0201(10) 0.0331(11) 0.0322(11) C53 0.0592(13) 0.0342(9) 0.0407(10) 0.0027(8) 0.0160(9) 0.0130(9) C54 0.0444(11) 0.0346(9) 0.0342(9) 0.0045(7) 0.0028(8) 0.0138(8) N1 0.0480(9) 0.0304(7) 0.0248(7) 0.0056(5) 0.0085(6) 0.0180(7) N2 0.0566(11) 0.0461(9) 0.0312(8) 0.0120(7) 0.0016(7) 0.0230(8) N3 0.0582(11) 0.0594(10) 0.0335(8) 0.0218(7) 0.0160(7) 0.0341(9) N4 0.0601(10) 0.0328(8) 0.0297(8) 0.0103(6) 0.0128(7) 0.0220(7) S1 0.0437(3) 0.0409(2) 0.0290(2) 0.01334(17) 0.01215(18) 0.0208(2) S2 0.0475(3) 0.0379(2) 0.0301(2) 0.00956(17) 0.00017(19) 0.0172(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 C1 C6 1.390(3) . ? C1 C2 1.392(2) . ? C1 N1 1.435(2) . ? C2 C3 1.390(2) . ? C2 H2A 0.9300 . ? C3 C4 1.383(3) . ? C3 H3A 0.9300 . ? C4 C5 1.385(3) . ? C4 H4A 0.9300 . ? C5 C6 1.393(2) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.392(2) . ? C7 C12 1.400(2) . ? C7 N1 1.417(2) . ? C8 C9 1.379(3) . ? C8 H8A 0.9300 . ? C9 C10 1.385(3) . ? C9 H9A 0.9300 . ? C10 C11 1.383(3) . ? C10 H10A 0.9300 . ? C11 C12 1.380(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.396(2) . ? C13 C18 1.398(2) . ? C13 N1 1.417(2) . ? C14 C15 1.384(2) . ? C14 H14A 0.9300 . ? C15 C16 1.398(2) . ? C15 H15A 0.9300 . ? C16 C17 1.394(2) . ? C16 C19 1.470(2) . ? C17 C18 1.382(2) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.367(2) . ? C19 S2 1.7383(18) . ? C20 C21 1.411(2) . ? C20 H20A 0.9300 . ? C21 C22 1.365(3) . ? C21 H21A 0.9300 . ? C22 C24 1.467(2) . ? C22 S2 1.7310(17) . ? C23 N2 1.333(2) . ? C23 C24 1.395(3) . ? C23 H23A 0.9300 . ? C24 C25 1.396(2) . ? C25 C26 1.377(3) . ? C25 H25A 0.9300 . ? C26 C27 1.387(3) . ? C26 H26A 0.9300 . ? C27 N2 1.349(2) . ? C27 C28 1.479(3) . ? C28 N3 1.347(2) . ? C28 C29 1.397(3) . ? C29 C30 1.373(3) . ? C29 H29A 0.9300 . ? C30 C31 1.403(2) . ? C30 H30A 0.9300 . ? C31 C32 1.394(2) . ? C31 C33 1.456(2) . ? C32 N3 1.330(2) . ? C32 H32A 0.9300 . ? C33 C34 1.364(2) . ? C33 S1 1.7369(16) . ? C34 C35 1.404(3) . ? C34 H34A 0.9300 . ? C35 C36 1.365(2) . ? C35 H35A 0.9300 . ? C36 C37 1.468(2) . ? C36 S1 1.7333(17) . ? C37 C38 1.398(2) . ? C37 C42 1.403(2) . ? C38 C39 1.385(2) . ? C38 H38A 0.9300 . ? C39 C40 1.386(2) . ? C39 H39A 0.9300 . ? C40 C41 1.400(2) . ? C40 N4 1.417(2) . ? C41 C42 1.381(2) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 C48 1.394(2) . ? C43 C44 1.394(2) . ? C43 N4 1.425(2) . ? C44 C45 1.386(3) . ? C44 H44A 0.9300 . ? C45 C46 1.380(3) . ? C45 H45A 0.9300 . ? C46 C47 1.380(3) . ? C46 H46A 0.9300 . ? C47 C48 1.388(3) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? C49 C50 1.388(3) . ? C49 C54 1.394(2) . ? C49 N4 1.424(2) . ? C50 C51 1.382(3) . ? C50 H50A 0.9300 . ? C51 C52 1.377(3) . ? C51 H51A 0.9300 . ? C52 C53 1.386(3) . ? C52 H52A 0.9300 . ? C53 C54 1.384(3) . ? C53 H53A 0.9300 . ? C54 H54A 0.9300 . ? 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 C6 C1 C2 119.55(16) . . ? C6 C1 N1 120.74(16) . . ? C2 C1 N1 119.71(16) . . ? C3 C2 C1 120.03(18) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C4 C3 C2 120.57(18) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 119.39(17) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C4 C5 C6 120.62(19) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C1 C6 C5 119.82(18) . . ? C1 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C8 C7 C12 118.14(15) . . ? C8 C7 N1 120.77(14) . . ? C12 C7 N1 121.09(15) . . ? C9 C8 C7 120.98(17) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C8 C9 C10 120.45(17) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 119.19(17) . . ? C11 C10 H10A 120.4 . . ? C9 C10 H10A 120.4 . . ? C12 C11 C10 120.70(18) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C7 120.53(17) . . ? C11 C12 H12A 119.7 . . ? C7 C12 H12A 119.7 . . ? C14 C13 C18 118.14(15) . . ? C14 C13 N1 122.83(15) . . ? C18 C13 N1 119.01(15) . . ? C15 C14 C13 120.26(16) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 121.96(16) . . ? C14 C15 H15A 119.0 . . ? C16 C15 H15A 119.0 . . ? C17 C16 C15 117.28(15) . . ? C17 C16 C19 121.96(15) . . ? C15 C16 C19 120.74(15) . . ? C18 C17 C16 121.29(15) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C13 121.07(15) . . ? C17 C18 H18A 119.5 . . ? C13 C18 H18A 119.5 . . ? C20 C19 C16 128.78(16) . . ? C20 C19 S2 110.08(13) . . ? C16 C19 S2 121.10(13) . . ? C19 C20 C21 113.48(17) . . ? C19 C20 H20A 123.3 . . ? C21 C20 H20A 123.3 . . ? C22 C21 C20 113.71(16) . . ? C22 C21 H21A 123.1 . . ? C20 C21 H21A 123.1 . . ? C21 C22 C24 126.88(16) . . ? C21 C22 S2 110.27(13) . . ? C24 C22 S2 122.56(14) . . ? N2 C23 C24 125.02(17) . . ? N2 C23 H23A 117.5 . . ? C24 C23 H23A 117.5 . . ? C23 C24 C25 116.29(17) . . ? C23 C24 C22 122.50(16) . . ? C25 C24 C22 121.01(17) . . ? C26 C25 C24 119.54(18) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C25 C26 C27 119.67(17) . . ? C25 C26 H26A 120.2 . . ? C27 C26 H26A 120.2 . . ? N2 C27 C26 121.95(17) . . ? N2 C27 C28 116.51(16) . . ? C26 C27 C28 121.41(16) . . ? N3 C28 C29 121.56(16) . . ? N3 C28 C27 117.01(16) . . ? C29 C28 C27 121.39(15) . . ? C30 C29 C28 119.63(16) . . ? C30 C29 H29A 120.2 . . ? C28 C29 H29A 120.2 . . ? C29 C30 C31 119.85(17) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 120.1 . . ? C32 C31 C30 116.00(16) . . ? C32 C31 C33 122.06(15) . . ? C30 C31 C33 121.93(16) . . ? N3 C32 C31 125.17(16) . . ? N3 C32 H32A 117.4 . . ? C31 C32 H32A 117.4 . . ? C34 C33 C31 128.43(15) . . ? C34 C33 S1 109.71(13) . . ? C31 C33 S1 121.86(13) . . ? C33 C34 C35 113.81(16) . . ? C33 C34 H34A 123.1 . . ? C35 C34 H34A 123.1 . . ? C36 C35 C34 114.09(17) . . ? C36 C35 H35A 123.0 . . ? C34 C35 H35A 123.0 . . ? C35 C36 C37 128.72(16) . . ? C35 C36 S1 109.66(13) . . ? C37 C36 S1 121.63(12) . . ? C38 C37 C42 117.55(15) . . ? C38 C37 C36 121.90(15) . . ? C42 C37 C36 120.55(15) . . ? C39 C38 C37 121.06(16) . . ? C39 C38 H38A 119.5 . . ? C37 C38 H38A 119.5 . . ? C38 C39 C40 120.91(15) . . ? C38 C39 H39A 119.5 . . ? C40 C39 H39A 119.5 . . ? C39 C40 C41 118.77(15) . . ? C39 C40 N4 120.61(15) . . ? C41 C40 N4 120.61(16) . . ? C42 C41 C40 120.18(17) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C41 C42 C37 121.51(16) . . ? C41 C42 H42A 119.2 . . ? C37 C42 H42A 119.2 . . ? C48 C43 C44 118.96(16) . . ? C48 C43 N4 120.20(15) . . ? C44 C43 N4 120.83(15) . . ? C45 C44 C43 120.00(16) . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C46 C45 C44 120.98(17) . . ? C46 C45 H45A 119.5 . . ? C44 C45 H45A 119.5 . . ? C45 C46 C47 119.02(17) . . ? C45 C46 H46A 120.5 . . ? C47 C46 H46A 120.5 . . ? C46 C47 C48 120.87(18) . . ? C46 C47 H47A 119.6 . . ? C48 C47 H47A 119.6 . . ? C47 C48 C43 120.00(17) . . ? C47 C48 H48A 120.0 . . ? C43 C48 H48A 120.0 . . ? C50 C49 C54 118.95(17) . . ? C50 C49 N4 120.91(16) . . ? C54 C49 N4 120.15(16) . . ? C51 C50 C49 120.28(19) . . ? C51 C50 H50A 119.9 . . ? C49 C50 H50A 119.9 . . ? C52 C51 C50 121.0(2) . . ? C52 C51 H51A 119.5 . . ? C50 C51 H51A 119.5 . . ? C51 C52 C53 118.95(18) . . ? C51 C52 H52A 120.5 . . ? C53 C52 H52A 120.5 . . ? C54 C53 C52 120.75(19) . . ? C54 C53 H53A 119.6 . . ? C52 C53 H53A 119.6 . . ? C53 C54 C49 120.07(18) . . ? C53 C54 H54A 120.0 . . ? C49 C54 H54A 120.0 . . ? C13 N1 C7 122.09(13) . . ? C13 N1 C1 117.68(13) . . ? C7 N1 C1 120.05(13) . . ? C23 N2 C27 117.30(17) . . ? C32 N3 C28 117.79(16) . . ? C40 N4 C49 120.08(13) . . ? C40 N4 C43 119.16(14) . . ? C49 N4 C43 119.89(14) . . ? C36 S1 C33 92.74(8) . . ? C22 S2 C19 92.45(9) . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 0.408 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.054