# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email chenzsh08@st.lzu.edu.cn _publ_contact_author_name 'Dr. Chen' loop_ _publ_author_name 'Yong-Ming Liang' 'Ying-Xiu Li' 'Hai-Xi Wang' 'Shaukat Ali' data_c2c _database_code_depnum_ccdc_archive 'CCDC 843867' #TrackingRef 'the compound 5 .cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H38 N4 O4 S2' _chemical_formula_weight 654.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.563(7) _cell_length_b 12.194(3) _cell_length_c 19.897(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.099(3) _cell_angle_gamma 90.00 _cell_volume 7488(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3579 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 22.79 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 0.183 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9557 _exptl_absorpt_correction_T_max 0.9609 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16221 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6776 _reflns_number_gt 3339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.2109P] 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 6776 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1302 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.2020 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 -0.072 0.250 316 58 ' ' 2 0.500 0.072 0.750 316 58 ' ' 3 0.308 0.083 0.327 9 0 ' ' 4 0.692 0.083 0.173 9 1 ' ' 5 0.000 0.428 0.250 316 58 ' ' 6 0.000 0.572 0.750 316 58 ' ' 7 0.192 0.417 0.673 9 1 ' ' 8 0.808 0.417 0.827 9 0 ' ' 9 0.192 0.583 0.173 9 1 ' ' 10 0.808 0.583 0.327 9 0 ' ' 11 0.308 0.917 0.827 9 0 ' ' 12 0.692 0.917 0.673 9 1 ' ' _platon_squeeze_details ; ; 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 0.21097(12) 0.2299(3) 0.58719(19) 0.0434(9) Uani 1 1 d . . . C2 C 0.24297(15) 0.3037(3) 0.5825(2) 0.0577(11) Uani 1 1 d . . . H2 H 0.2362 0.3736 0.5648 0.069 Uiso 1 1 calc R . . C3 C 0.28497(15) 0.2721(4) 0.6046(2) 0.0646(13) Uani 1 1 d . . . H3 H 0.3070 0.3220 0.6026 0.077 Uiso 1 1 calc R . . C4 C 0.29586(13) 0.1682(4) 0.6297(2) 0.0604(12) Uani 1 1 d . . . H4 H 0.3248 0.1478 0.6427 0.073 Uiso 1 1 calc R . . C5 C 0.26330(12) 0.0935(3) 0.63564(19) 0.0500(10) Uani 1 1 d . . . H5 H 0.2702 0.0235 0.6530 0.060 Uiso 1 1 calc R . . C6 C 0.22066(12) 0.1261(3) 0.61511(18) 0.0410(9) Uani 1 1 d . . . C7 C 0.17911(11) 0.0631(3) 0.61317(18) 0.0381(9) Uani 1 1 d . . . C8 C 0.14639(11) 0.1366(3) 0.56375(17) 0.0384(9) Uani 1 1 d . . . H8 H 0.1184 0.1398 0.5777 0.046 Uiso 1 1 calc R . . C9 C 0.17867(12) -0.0461(3) 0.5760(2) 0.0453(10) Uani 1 1 d . . . H9A H 0.2058 -0.0851 0.5913 0.054 Uiso 1 1 calc R . . H9B H 0.1550 -0.0920 0.5836 0.054 Uiso 1 1 calc R . . C10 C 0.17253(12) -0.0142(3) 0.5010(2) 0.0481(10) Uani 1 1 d . . . H10A H 0.1997 0.0074 0.4896 0.058 Uiso 1 1 calc R . . H10B H 0.1599 -0.0738 0.4711 0.058 Uiso 1 1 calc R . . C11 C 0.07244(12) -0.0459(3) 0.4420(2) 0.0477(10) Uani 1 1 d . . . C12 C 0.07330(14) -0.1265(4) 0.3949(2) 0.0691(13) Uani 1 1 d . . . H12 H 0.0893 -0.1168 0.3610 0.083 Uiso 1 1 calc R . . C13 C 0.05049(17) -0.2228(4) 0.3973(3) 0.0822(15) Uani 1 1 d . . . H13 H 0.0520 -0.2781 0.3657 0.099 Uiso 1 1 calc R . . C14 C 0.02587(14) -0.2379(4) 0.4452(3) 0.0675(13) Uani 1 1 d . . . C15 C 0.02618(13) -0.1577(4) 0.4943(2) 0.0658(12) Uani 1 1 d . . . H15 H 0.0104 -0.1685 0.5283 0.079 Uiso 1 1 calc R . . C16 C 0.04931(13) -0.0626(4) 0.4939(2) 0.0554(11) Uani 1 1 d . . . H16 H 0.0496 -0.0098 0.5278 0.066 Uiso 1 1 calc R . . C17 C -0.00081(18) -0.3407(5) 0.4459(3) 0.107(2) Uani 1 1 d . . . H17A H -0.0236 -0.3267 0.4699 0.161 Uiso 1 1 calc R . . H17B H 0.0174 -0.3985 0.4686 0.161 Uiso 1 1 calc R . . H17C H -0.0131 -0.3623 0.3995 0.161 Uiso 1 1 calc R . . C18 C 0.14579(15) 0.3343(3) 0.5293(3) 0.0747(14) Uani 1 1 d . . . H18A H 0.1610 0.4001 0.5465 0.112 Uiso 1 1 calc R . . H18B H 0.1163 0.3393 0.5345 0.112 Uiso 1 1 calc R . . H18C H 0.1464 0.3254 0.4816 0.112 Uiso 1 1 calc R . . C19 C 0.09620(14) 0.1092(4) 0.6951(2) 0.0580(11) Uani 1 1 d . . . C20 C 0.05239(15) 0.0991(5) 0.6966(2) 0.0773(15) Uani 1 1 d . . . H20 H 0.0361 0.1589 0.7055 0.093 Uiso 1 1 calc R . . C21 C 0.03423(16) -0.0041(7) 0.6841(2) 0.0912(19) Uani 1 1 d . . . H21 H 0.0047 -0.0123 0.6825 0.109 Uiso 1 1 calc R . . C22 C 0.05818(17) -0.0963(5) 0.6739(2) 0.0818(16) Uani 1 1 d . . . H22 H 0.0452 -0.1651 0.6675 0.098 Uiso 1 1 calc R . . C23 C 0.10128(14) -0.0832(4) 0.6734(2) 0.0618(12) Uani 1 1 d . . . H23 H 0.1178 -0.1438 0.6667 0.074 Uiso 1 1 calc R . . C24 C 0.12009(12) 0.0179(3) 0.68268(18) 0.0448(9) Uani 1 1 d . . . C25 C 0.16704(11) 0.0537(3) 0.68597(18) 0.0391(9) Uani 1 1 d . . . C26 C 0.16674(13) 0.1685(3) 0.72093(18) 0.0459(9) Uani 1 1 d . . . H26 H 0.1849 0.2213 0.7028 0.055 Uiso 1 1 calc R . . C27 C 0.19165(13) 0.0260(3) 0.8070(2) 0.0519(10) Uani 1 1 d . . . H27A H 0.1668 -0.0089 0.8194 0.062 Uiso 1 1 calc R . . H27B H 0.2170 0.0130 0.8431 0.062 Uiso 1 1 calc R . . C28 C 0.19849(12) -0.0149(3) 0.73891(19) 0.0472(10) Uani 1 1 d . . . H28A H 0.1917 -0.0924 0.7333 0.057 Uiso 1 1 calc R . . H28B H 0.2282 -0.0034 0.7345 0.057 Uiso 1 1 calc R . . C29 C 0.26533(14) 0.1903(3) 0.8652(2) 0.0564(11) Uani 1 1 d . . . C30 C 0.2869(2) 0.1703(3) 0.9318(2) 0.0749(14) Uani 1 1 d . . . H30 H 0.2723 0.1746 0.9677 0.090 Uiso 1 1 calc R . . C31 C 0.3302(2) 0.1439(4) 0.9446(3) 0.0899(18) Uani 1 1 d . . . H31 H 0.3450 0.1338 0.9898 0.108 Uiso 1 1 calc R . . C32 C 0.35241(19) 0.1320(4) 0.8920(4) 0.0834(16) Uani 1 1 d . . . C33 C 0.32929(18) 0.1532(4) 0.8258(3) 0.0848(16) Uani 1 1 d . . . H33 H 0.3435 0.1475 0.7895 0.102 Uiso 1 1 calc R . . C34 C 0.28703(16) 0.1815(4) 0.8120(2) 0.0712(13) Uani 1 1 d . . . H34 H 0.2726 0.1950 0.7670 0.085 Uiso 1 1 calc R . . C35 C 0.39942(19) 0.1024(5) 0.9078(4) 0.129(2) Uani 1 1 d . . . H35A H 0.4081 0.0823 0.9554 0.194 Uiso 1 1 calc R . . H35B H 0.4162 0.1641 0.8986 0.194 Uiso 1 1 calc R . . H35C H 0.4042 0.0417 0.8796 0.194 Uiso 1 1 calc R . . C36 C 0.10849(18) 0.3025(4) 0.7310(3) 0.0908(17) Uani 1 1 d . . . H36A H 0.0793 0.3190 0.7080 0.136 Uiso 1 1 calc R . . H36B H 0.1274 0.3602 0.7225 0.136 Uiso 1 1 calc R . . H36C H 0.1099 0.2966 0.7795 0.136 Uiso 1 1 calc R . . N1 N 0.16619(10) 0.2420(2) 0.56723(16) 0.0470(8) Uani 1 1 d . . . N2 N 0.14240(9) 0.0795(2) 0.49624(15) 0.0435(8) Uani 1 1 d . . . N3 N 0.12165(12) 0.2014(3) 0.70579(17) 0.0580(9) Uani 1 1 d . . . N4 N 0.18411(11) 0.1452(2) 0.79452(15) 0.0546(9) Uani 1 1 d . . . O1 O 0.11010(9) 0.0845(2) 0.37207(13) 0.0624(8) Uani 1 1 d . . . O2 O 0.07212(8) 0.1648(2) 0.45567(14) 0.0595(8) Uani 1 1 d . . . O3 O 0.20726(11) 0.3353(2) 0.81137(16) 0.0764(9) Uani 1 1 d . . . O4 O 0.19610(11) 0.2269(3) 0.91113(15) 0.0808(10) Uani 1 1 d . . . S1 S 0.09871(3) 0.08022(9) 0.43754(5) 0.0481(3) Uani 1 1 d . . . S2 S 0.21067(4) 0.23318(9) 0.84741(6) 0.0623(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 0.053(2) 0.037(2) 0.042(2) -0.0072(17) 0.0157(18) -0.0094(19) C2 0.075(3) 0.046(2) 0.055(3) 0.000(2) 0.020(2) -0.017(2) C3 0.067(3) 0.067(3) 0.066(3) -0.010(2) 0.028(2) -0.030(3) C4 0.041(2) 0.085(4) 0.057(3) -0.007(2) 0.014(2) -0.018(2) C5 0.045(2) 0.058(3) 0.048(2) 0.0010(19) 0.0124(18) 0.003(2) C6 0.047(2) 0.043(2) 0.037(2) -0.0042(17) 0.0166(17) -0.0043(18) C7 0.041(2) 0.034(2) 0.041(2) -0.0023(16) 0.0143(16) -0.0012(16) C8 0.043(2) 0.038(2) 0.036(2) -0.0018(16) 0.0153(16) -0.0029(17) C9 0.045(2) 0.035(2) 0.058(3) -0.0037(18) 0.0144(18) -0.0026(17) C10 0.046(2) 0.047(2) 0.053(3) -0.0125(19) 0.0134(18) 0.0048(19) C11 0.037(2) 0.062(3) 0.042(2) -0.0050(19) 0.0054(18) -0.0036(19) C12 0.060(3) 0.090(4) 0.061(3) -0.023(3) 0.022(2) -0.003(3) C13 0.078(3) 0.074(4) 0.097(4) -0.037(3) 0.025(3) -0.016(3) C14 0.052(3) 0.063(3) 0.083(4) 0.001(3) 0.004(2) -0.009(2) C15 0.052(3) 0.079(4) 0.069(3) 0.004(3) 0.020(2) -0.007(3) C16 0.055(2) 0.059(3) 0.053(3) -0.001(2) 0.014(2) -0.001(2) C17 0.089(4) 0.101(4) 0.127(5) -0.013(4) 0.013(3) -0.043(4) C18 0.080(3) 0.045(3) 0.099(4) 0.012(3) 0.020(3) 0.007(2) C19 0.055(3) 0.080(3) 0.040(2) 0.006(2) 0.0122(19) 0.012(3) C20 0.050(3) 0.132(5) 0.055(3) 0.005(3) 0.022(2) 0.007(3) C21 0.049(3) 0.175(7) 0.054(3) 0.012(4) 0.020(2) -0.019(4) C22 0.066(3) 0.120(5) 0.062(3) 0.008(3) 0.019(3) -0.040(3) C23 0.061(3) 0.077(3) 0.051(3) 0.001(2) 0.020(2) -0.022(2) C24 0.046(2) 0.053(3) 0.039(2) 0.0012(18) 0.0154(17) -0.003(2) C25 0.042(2) 0.036(2) 0.043(2) 0.0001(16) 0.0160(17) -0.0024(17) C26 0.063(3) 0.043(2) 0.034(2) 0.0011(17) 0.0143(18) 0.000(2) C27 0.065(3) 0.044(2) 0.045(2) 0.0058(19) 0.010(2) -0.015(2) C28 0.051(2) 0.040(2) 0.049(2) 0.0062(18) 0.0067(18) -0.0030(18) C29 0.079(3) 0.044(2) 0.045(3) -0.0063(19) 0.009(2) -0.021(2) C30 0.125(5) 0.045(3) 0.051(3) -0.008(2) 0.009(3) -0.013(3) C31 0.117(5) 0.052(3) 0.081(4) -0.006(3) -0.025(4) -0.014(3) C32 0.093(4) 0.054(3) 0.095(4) -0.005(3) 0.001(4) -0.028(3) C33 0.085(4) 0.089(4) 0.082(4) -0.011(3) 0.020(3) -0.029(3) C34 0.073(3) 0.085(4) 0.055(3) -0.006(3) 0.012(3) -0.031(3) C35 0.086(4) 0.114(5) 0.166(7) 0.013(5) -0.025(4) -0.014(4) C36 0.116(4) 0.068(3) 0.091(4) -0.004(3) 0.028(3) 0.038(3) N1 0.057(2) 0.0330(18) 0.051(2) 0.0053(14) 0.0118(16) -0.0004(15) N2 0.0397(17) 0.0485(19) 0.0449(19) -0.0090(15) 0.0148(14) 0.0057(15) N3 0.067(2) 0.052(2) 0.059(2) -0.0060(17) 0.0220(18) 0.0134(19) N4 0.085(2) 0.0388(19) 0.0384(19) 0.0000(15) 0.0099(17) -0.0115(18) O1 0.0603(17) 0.091(2) 0.0381(16) 0.0066(15) 0.0151(13) -0.0055(16) O2 0.0500(16) 0.0617(18) 0.0685(19) 0.0047(15) 0.0164(14) 0.0105(14) O3 0.115(3) 0.0443(18) 0.070(2) -0.0058(15) 0.0194(18) -0.0144(17) O4 0.115(3) 0.086(2) 0.0463(19) -0.0137(16) 0.0297(17) -0.015(2) S1 0.0427(6) 0.0600(7) 0.0429(6) 0.0012(5) 0.0120(4) 0.0004(5) S2 0.0960(9) 0.0483(7) 0.0443(7) -0.0086(5) 0.0190(6) -0.0165(6) _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 1.371(5) . ? C1 C6 1.390(5) . ? C1 N1 1.394(5) . ? C2 C3 1.362(6) . ? C2 H2 0.9300 . ? C3 C4 1.379(6) . ? C3 H3 0.9300 . ? C4 C5 1.396(5) . ? C4 H4 0.9300 . ? C5 C6 1.381(5) . ? C5 H5 0.9300 . ? C6 C7 1.513(5) . ? C7 C9 1.522(5) . ? C7 C8 1.553(5) . ? C7 C25 1.577(5) . ? C8 N1 1.425(4) . ? C8 N2 1.495(4) . ? C8 H8 0.9800 . ? C9 C10 1.514(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.477(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.363(6) . ? C11 C16 1.400(5) . ? C11 S1 1.758(4) . ? C12 C13 1.383(6) . ? C12 H12 0.9300 . ? C13 C14 1.363(7) . ? C13 H13 0.9300 . ? C14 C15 1.380(6) . ? C14 C17 1.512(6) . ? C15 C16 1.372(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N1 1.430(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.372(5) . ? C19 C20 1.395(6) . ? C19 C24 1.396(5) . ? C20 C21 1.383(8) . ? C20 H20 0.9300 . ? C21 C22 1.393(7) . ? C21 H21 0.9300 . ? C22 C23 1.372(6) . ? C22 H22 0.9300 . ? C23 C24 1.364(5) . ? C23 H23 0.9300 . ? C24 C25 1.533(5) . ? C25 C28 1.535(5) . ? C25 C26 1.564(5) . ? C26 N3 1.448(5) . ? C26 N4 1.479(4) . ? C26 H26 0.9800 . ? C27 N4 1.486(5) . ? C27 C28 1.501(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.379(6) . ? C29 C34 1.380(6) . ? C29 S2 1.766(5) . ? C30 C31 1.375(7) . ? C30 H30 0.9300 . ? C31 C32 1.383(7) . ? C31 H31 0.9300 . ? C32 C33 1.390(7) . ? C32 C35 1.495(8) . ? C33 C34 1.350(7) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 N3 1.426(5) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? N2 S1 1.610(3) . ? N4 S2 1.609(3) . ? O1 S1 1.423(3) . ? O2 S1 1.423(3) . ? O3 S2 1.429(3) . ? O4 S2 1.438(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 121.4(4) . . ? C2 C1 N1 128.9(4) . . ? C6 C1 N1 109.6(3) . . ? C3 C2 C1 118.2(4) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 121.9(4) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C3 C4 C5 119.9(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 118.5(4) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 C1 119.9(3) . . ? C5 C6 C7 130.4(3) . . ? C1 C6 C7 109.6(3) . . ? C6 C7 C9 112.1(3) . . ? C6 C7 C8 100.4(3) . . ? C9 C7 C8 105.1(3) . . ? C6 C7 C25 112.8(3) . . ? C9 C7 C25 113.9(3) . . ? C8 C7 C25 111.5(3) . . ? N1 C8 N2 114.7(3) . . ? N1 C8 C7 105.3(3) . . ? N2 C8 C7 102.7(3) . . ? N1 C8 H8 111.2 . . ? N2 C8 H8 111.2 . . ? C7 C8 H8 111.2 . . ? C10 C9 C7 103.9(3) . . ? C10 C9 H9A 111.0 . . ? C7 C9 H9A 111.0 . . ? C10 C9 H9B 111.0 . . ? C7 C9 H9B 111.0 . . ? H9A C9 H9B 109.0 . . ? N2 C10 C9 102.1(3) . . ? N2 C10 H10A 111.3 . . ? C9 C10 H10A 111.3 . . ? N2 C10 H10B 111.3 . . ? C9 C10 H10B 111.3 . . ? H10A C10 H10B 109.2 . . ? C12 C11 C16 119.4(4) . . ? C12 C11 S1 121.3(3) . . ? C16 C11 S1 119.2(3) . . ? C11 C12 C13 120.2(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 121.1(4) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 118.6(4) . . ? C13 C14 C17 121.2(5) . . ? C15 C14 C17 120.2(5) . . ? C16 C15 C14 121.4(4) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C11 119.2(4) . . ? C15 C16 H16 120.4 . . ? C11 C16 H16 120.4 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 H18A 109.5 . . ? N1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 128.3(5) . . ? N3 C19 C24 111.1(4) . . ? C20 C19 C24 120.5(5) . . ? C21 C20 C19 116.9(5) . . ? C21 C20 H20 121.6 . . ? C19 C20 H20 121.6 . . ? C20 C21 C22 122.9(5) . . ? C20 C21 H21 118.6 . . ? C22 C21 H21 118.6 . . ? C23 C22 C21 118.5(5) . . ? C23 C22 H22 120.8 . . ? C21 C22 H22 120.8 . . ? C24 C23 C22 120.6(5) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C19 120.6(4) . . ? C23 C24 C25 130.8(4) . . ? C19 C24 C25 108.6(3) . . ? C24 C25 C28 110.7(3) . . ? C24 C25 C26 100.3(3) . . ? C28 C25 C26 104.2(3) . . ? C24 C25 C7 113.5(3) . . ? C28 C25 C7 115.1(3) . . ? C26 C25 C7 111.7(3) . . ? N3 C26 N4 113.8(3) . . ? N3 C26 C25 104.6(3) . . ? N4 C26 C25 103.5(3) . . ? N3 C26 H26 111.5 . . ? N4 C26 H26 111.5 . . ? C25 C26 H26 111.5 . . ? N4 C27 C28 102.9(3) . . ? N4 C27 H27A 111.2 . . ? C28 C27 H27A 111.2 . . ? N4 C27 H27B 111.2 . . ? C28 C27 H27B 111.2 . . ? H27A C27 H27B 109.1 . . ? C27 C28 C25 104.1(3) . . ? C27 C28 H28A 110.9 . . ? C25 C28 H28A 110.9 . . ? C27 C28 H28B 110.9 . . ? C25 C28 H28B 110.9 . . ? H28A C28 H28B 109.0 . . ? C30 C29 C34 119.9(5) . . ? C30 C29 S2 120.7(4) . . ? C34 C29 S2 119.4(3) . . ? C31 C30 C29 119.5(5) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 121.7(5) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C31 C32 C33 116.7(5) . . ? C31 C32 C35 120.2(6) . . ? C33 C32 C35 123.0(6) . . ? C34 C33 C32 122.7(5) . . ? C34 C33 H33 118.6 . . ? C32 C33 H33 118.6 . . ? C33 C34 C29 119.5(5) . . ? C33 C34 H34 120.3 . . ? C29 C34 H34 120.3 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C1 N1 C8 109.0(3) . . ? C1 N1 C18 123.5(3) . . ? C8 N1 C18 122.7(3) . . ? C10 N2 C8 111.8(3) . . ? C10 N2 S1 119.5(2) . . ? C8 N2 S1 123.2(2) . . ? C19 N3 C36 124.0(4) . . ? C19 N3 C26 108.9(3) . . ? C36 N3 C26 120.8(4) . . ? C26 N4 C27 111.5(3) . . ? C26 N4 S2 123.6(2) . . ? C27 N4 S2 120.0(3) . . ? O2 S1 O1 118.79(17) . . ? O2 S1 N2 106.31(16) . . ? O1 S1 N2 108.79(16) . . ? O2 S1 C11 108.17(18) . . ? O1 S1 C11 106.84(18) . . ? N2 S1 C11 107.48(17) . . ? O3 S2 O4 118.9(2) . . ? O3 S2 N4 106.15(18) . . ? O4 S2 N4 108.79(18) . . ? O3 S2 C29 109.0(2) . . ? O4 S2 C29 106.7(2) . . ? N4 S2 C29 106.67(19) . . ? 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 C6 C1 C2 C3 1.5(6) . . . . ? N1 C1 C2 C3 -178.8(4) . . . . ? C1 C2 C3 C4 1.4(6) . . . . ? C2 C3 C4 C5 -2.6(7) . . . . ? C3 C4 C5 C6 0.8(6) . . . . ? C4 C5 C6 C1 2.1(5) . . . . ? C4 C5 C6 C7 177.7(3) . . . . ? C2 C1 C6 C5 -3.3(5) . . . . ? N1 C1 C6 C5 177.0(3) . . . . ? C2 C1 C6 C7 -179.7(3) . . . . ? N1 C1 C6 C7 0.6(4) . . . . ? C5 C6 C7 C9 -51.2(5) . . . . ? C1 C6 C7 C9 124.7(3) . . . . ? C5 C6 C7 C8 -162.3(4) . . . . ? C1 C6 C7 C8 13.6(4) . . . . ? C5 C6 C7 C25 78.9(4) . . . . ? C1 C6 C7 C25 -105.2(3) . . . . ? C6 C7 C8 N1 -22.6(3) . . . . ? C9 C7 C8 N1 -139.0(3) . . . . ? C25 C7 C8 N1 97.1(3) . . . . ? C6 C7 C8 N2 97.7(3) . . . . ? C9 C7 C8 N2 -18.7(3) . . . . ? C25 C7 C8 N2 -142.5(3) . . . . ? C6 C7 C9 C10 -72.9(4) . . . . ? C8 C7 C9 C10 35.2(4) . . . . ? C25 C7 C9 C10 157.5(3) . . . . ? C7 C9 C10 N2 -37.2(4) . . . . ? C16 C11 C12 C13 1.8(7) . . . . ? S1 C11 C12 C13 -176.6(4) . . . . ? C11 C12 C13 C14 1.9(8) . . . . ? C12 C13 C14 C15 -4.0(8) . . . . ? C12 C13 C14 C17 177.0(5) . . . . ? C13 C14 C15 C16 2.5(7) . . . . ? C17 C14 C15 C16 -178.5(4) . . . . ? C14 C15 C16 C11 1.1(6) . . . . ? C12 C11 C16 C15 -3.2(6) . . . . ? S1 C11 C16 C15 175.2(3) . . . . ? N3 C19 C20 C21 -179.8(4) . . . . ? C24 C19 C20 C21 -1.1(6) . . . . ? C19 C20 C21 C22 3.2(7) . . . . ? C20 C21 C22 C23 -2.7(7) . . . . ? C21 C22 C23 C24 -0.1(7) . . . . ? C22 C23 C24 C19 2.1(6) . . . . ? C22 C23 C24 C25 178.4(4) . . . . ? N3 C19 C24 C23 177.4(4) . . . . ? C20 C19 C24 C23 -1.5(6) . . . . ? N3 C19 C24 C25 0.3(4) . . . . ? C20 C19 C24 C25 -178.6(3) . . . . ? C23 C24 C25 C28 -52.6(5) . . . . ? C19 C24 C25 C28 124.1(3) . . . . ? C23 C24 C25 C26 -162.2(4) . . . . ? C19 C24 C25 C26 14.5(4) . . . . ? C23 C24 C25 C7 78.6(5) . . . . ? C19 C24 C25 C7 -104.7(3) . . . . ? C6 C7 C25 C24 164.8(3) . . . . ? C9 C7 C25 C24 -66.0(4) . . . . ? C8 C7 C25 C24 52.7(4) . . . . ? C6 C7 C25 C28 -66.2(4) . . . . ? C9 C7 C25 C28 63.0(4) . . . . ? C8 C7 C25 C28 -178.3(3) . . . . ? C6 C7 C25 C26 52.4(4) . . . . ? C9 C7 C25 C26 -178.4(3) . . . . ? C8 C7 C25 C26 -59.7(4) . . . . ? C24 C25 C26 N3 -23.4(3) . . . . ? C28 C25 C26 N3 -138.0(3) . . . . ? C7 C25 C26 N3 97.1(3) . . . . ? C24 C25 C26 N4 96.0(3) . . . . ? C28 C25 C26 N4 -18.6(4) . . . . ? C7 C25 C26 N4 -143.5(3) . . . . ? N4 C27 C28 C25 -36.5(4) . . . . ? C24 C25 C28 C27 -72.5(4) . . . . ? C26 C25 C28 C27 34.5(4) . . . . ? C7 C25 C28 C27 157.2(3) . . . . ? C34 C29 C30 C31 1.3(6) . . . . ? S2 C29 C30 C31 -175.8(3) . . . . ? C29 C30 C31 C32 -2.9(7) . . . . ? C30 C31 C32 C33 2.9(7) . . . . ? C30 C31 C32 C35 -179.5(5) . . . . ? C31 C32 C33 C34 -1.5(7) . . . . ? C35 C32 C33 C34 -179.0(5) . . . . ? C32 C33 C34 C29 0.0(8) . . . . ? C30 C29 C34 C33 0.1(7) . . . . ? S2 C29 C34 C33 177.3(4) . . . . ? C2 C1 N1 C8 163.9(4) . . . . ? C6 C1 N1 C8 -16.4(4) . . . . ? C2 C1 N1 C18 8.0(6) . . . . ? C6 C1 N1 C18 -172.3(4) . . . . ? N2 C8 N1 C1 -87.3(3) . . . . ? C7 C8 N1 C1 24.8(4) . . . . ? N2 C8 N1 C18 68.8(5) . . . . ? C7 C8 N1 C18 -179.1(3) . . . . ? C9 C10 N2 C8 26.5(4) . . . . ? C9 C10 N2 S1 -128.2(3) . . . . ? N1 C8 N2 C10 108.7(3) . . . . ? C7 C8 N2 C10 -4.9(4) . . . . ? N1 C8 N2 S1 -97.7(3) . . . . ? C7 C8 N2 S1 148.6(3) . . . . ? C20 C19 N3 C36 9.9(7) . . . . ? C24 C19 N3 C36 -168.9(4) . . . . ? C20 C19 N3 C26 162.0(4) . . . . ? C24 C19 N3 C26 -16.8(4) . . . . ? N4 C26 N3 C19 -86.7(4) . . . . ? C25 C26 N3 C19 25.6(4) . . . . ? N4 C26 N3 C36 66.4(5) . . . . ? C25 C26 N3 C36 178.7(4) . . . . ? N3 C26 N4 C27 108.8(4) . . . . ? C25 C26 N4 C27 -4.1(4) . . . . ? N3 C26 N4 S2 -96.2(4) . . . . ? C25 C26 N4 S2 150.8(3) . . . . ? C28 C27 N4 C26 25.7(4) . . . . ? C28 C27 N4 S2 -130.3(3) . . . . ? C10 N2 S1 O2 166.5(3) . . . . ? C8 N2 S1 O2 14.8(3) . . . . ? C10 N2 S1 O1 -64.5(3) . . . . ? C8 N2 S1 O1 143.8(3) . . . . ? C10 N2 S1 C11 50.8(3) . . . . ? C8 N2 S1 C11 -100.8(3) . . . . ? C12 C11 S1 O2 141.3(3) . . . . ? C16 C11 S1 O2 -37.1(3) . . . . ? C12 C11 S1 O1 12.3(4) . . . . ? C16 C11 S1 O1 -166.1(3) . . . . ? C12 C11 S1 N2 -104.3(4) . . . . ? C16 C11 S1 N2 77.3(3) . . . . ? C26 N4 S2 O3 8.7(4) . . . . ? C27 N4 S2 O3 161.6(3) . . . . ? C26 N4 S2 O4 137.8(3) . . . . ? C27 N4 S2 O4 -69.3(3) . . . . ? C26 N4 S2 C29 -107.5(3) . . . . ? C27 N4 S2 C29 45.5(3) . . . . ? C30 C29 S2 O3 122.8(3) . . . . ? C34 C29 S2 O3 -54.4(4) . . . . ? C30 C29 S2 O4 -6.8(4) . . . . ? C34 C29 S2 O4 176.0(3) . . . . ? C30 C29 S2 N4 -123.0(3) . . . . ? C34 C29 S2 N4 59.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.715 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.063 # Attachment 'the compound 7.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 843868' #TrackingRef 'the compound 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 N4' _chemical_formula_weight 374.53 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.442(8) _cell_length_b 16.060(5) _cell_length_c 13.506(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.289(3) _cell_angle_gamma 90.00 _cell_volume 6169(3) _cell_formula_units_Z 12 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2567 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 20.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9821 _exptl_absorpt_correction_T_max 0.9842 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20537 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.49 _reflns_number_total 5714 _reflns_number_gt 3055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+1.4508P] 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 5714 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1176 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 0.40939(8) 0.09567(14) 0.01695(18) 0.0440(6) Uani 1 1 d . . . C2 C 0.42776(9) 0.17153(15) -0.0128(2) 0.0580(7) Uani 1 1 d . . . H2 H 0.4519 0.1968 0.0229 0.070 Uiso 1 1 calc R . . C3 C 0.40946(10) 0.20887(17) -0.0968(2) 0.0670(8) Uani 1 1 d . . . H3 H 0.4217 0.2594 -0.1183 0.080 Uiso 1 1 calc R . . C4 C 0.37348(10) 0.17226(17) -0.1489(2) 0.0672(8) Uani 1 1 d . . . H4 H 0.3615 0.1982 -0.2053 0.081 Uiso 1 1 calc R . . C5 C 0.35483(9) 0.09699(16) -0.11815(19) 0.0555(7) Uani 1 1 d . . . H5 H 0.3303 0.0725 -0.1535 0.067 Uiso 1 1 calc R . . C6 C 0.37275(7) 0.05847(14) -0.03468(17) 0.0410(6) Uani 1 1 d . . . C7 C 0.35950(7) -0.02353(13) 0.01268(17) 0.0411(6) Uani 1 1 d . . . C8 C 0.37413(8) -0.09772(14) -0.05391(19) 0.0522(7) Uani 1 1 d . . . H8A H 0.3534 -0.1450 -0.0444 0.063 Uiso 1 1 calc R . . H8B H 0.3737 -0.0821 -0.1233 0.063 Uiso 1 1 calc R . . C9 C 0.42343(9) -0.11744(16) -0.0194(2) 0.0605(7) Uani 1 1 d . . . H9A H 0.4322 -0.1740 -0.0363 0.073 Uiso 1 1 calc R . . H9B H 0.4461 -0.0791 -0.0475 0.073 Uiso 1 1 calc R . . C10 C 0.39492(7) -0.02879(14) 0.10203(18) 0.0460(6) Uani 1 1 d . . . H10 H 0.3779 -0.0299 0.1649 0.055 Uiso 1 1 calc R . . C11 C 0.46326(9) -0.11577(18) 0.1425(2) 0.0778(9) Uani 1 1 d . . . H11A H 0.4757 -0.1707 0.1326 0.117 Uiso 1 1 calc R . . H11B H 0.4572 -0.1074 0.2117 0.117 Uiso 1 1 calc R . . H11C H 0.4856 -0.0752 0.1202 0.117 Uiso 1 1 calc R . . C12 C 0.44441(10) 0.08377(18) 0.1830(2) 0.0747(9) Uani 1 1 d . . . H12A H 0.4737 0.1100 0.1664 0.112 Uiso 1 1 calc R . . H12B H 0.4499 0.0414 0.2319 0.112 Uiso 1 1 calc R . . H12C H 0.4232 0.1247 0.2090 0.112 Uiso 1 1 calc R . . C13 C 0.24950(8) 0.07890(16) 0.0328(2) 0.0521(7) Uani 1 1 d . . . C14 C 0.22640(10) 0.15220(17) 0.0566(3) 0.0724(9) Uani 1 1 d . . . H14 H 0.2006 0.1702 0.0199 0.087 Uiso 1 1 calc R . . C15 C 0.24288(12) 0.19774(19) 0.1362(3) 0.0824(10) Uani 1 1 d . . . H15 H 0.2279 0.2473 0.1528 0.099 Uiso 1 1 calc R . . C16 C 0.28051(11) 0.17204(19) 0.1911(3) 0.0812(10) Uani 1 1 d . . . H16 H 0.2907 0.2035 0.2449 0.097 Uiso 1 1 calc R . . C17 C 0.30352(9) 0.09882(16) 0.1665(2) 0.0606(7) Uani 1 1 d . . . H17 H 0.3292 0.0811 0.2037 0.073 Uiso 1 1 calc R . . C18 C 0.28833(8) 0.05253(14) 0.08707(18) 0.0449(6) Uani 1 1 d . . . C19 C 0.30700(7) -0.02858(14) 0.04527(17) 0.0416(6) Uani 1 1 d . . . C20 C 0.29793(8) -0.10123(15) 0.11826(19) 0.0534(7) Uani 1 1 d . . . H20A H 0.3215 -0.1445 0.1112 0.064 Uiso 1 1 calc R . . H20B H 0.2980 -0.0817 0.1862 0.064 Uiso 1 1 calc R . . C21 C 0.25014(9) -0.13240(15) 0.0886(2) 0.0597(7) Uani 1 1 d . . . H21A H 0.2451 -0.1890 0.1112 0.072 Uiso 1 1 calc R . . H21B H 0.2255 -0.0969 0.1143 0.072 Uiso 1 1 calc R . . C22 C 0.27217(8) -0.04697(15) -0.04155(18) 0.0484(6) Uani 1 1 d . . . H22 H 0.2891 -0.0490 -0.1046 0.058 Uiso 1 1 calc R . . C23 C 0.20877(9) -0.14890(17) -0.0693(2) 0.0748(9) Uani 1 1 d . . . H23A H 0.1993 -0.2043 -0.0514 0.112 Uiso 1 1 calc R . . H23B H 0.2134 -0.1460 -0.1395 0.112 Uiso 1 1 calc R . . H23C H 0.1847 -0.1101 -0.0503 0.112 Uiso 1 1 calc R . . C24 C 0.21450(10) 0.04799(19) -0.1312(2) 0.0878(10) Uani 1 1 d . . . H24A H 0.1812 0.0482 -0.1202 0.132 Uiso 1 1 calc R . . H24B H 0.2218 0.0097 -0.1835 0.132 Uiso 1 1 calc R . . H24C H 0.2246 0.1029 -0.1495 0.132 Uiso 1 1 calc R . . C25 C 0.08137(8) -0.04628(14) 0.76148(18) 0.0438(6) Uani 1 1 d . . . C26 C 0.10206(9) -0.12176(15) 0.7851(2) 0.0560(7) Uani 1 1 d . . . H26 H 0.1287 -0.1401 0.7520 0.067 Uiso 1 1 calc R . . C27 C 0.08190(10) -0.16951(15) 0.8595(2) 0.0614(8) Uani 1 1 d . . . H27 H 0.0951 -0.2206 0.8761 0.074 Uiso 1 1 calc R . . C28 C 0.04282(10) -0.14230(15) 0.9087(2) 0.0600(7) Uani 1 1 d . . . H28 H 0.0298 -0.1750 0.9584 0.072 Uiso 1 1 calc R . . C29 C 0.02246(9) -0.06651(14) 0.88507(18) 0.0496(6) Uani 1 1 d . . . H29 H -0.0041 -0.0483 0.9187 0.060 Uiso 1 1 calc R . . C30 C 0.04178(8) -0.01833(13) 0.81142(17) 0.0397(6) Uani 1 1 d . . . C31 C 0.02601(7) 0.06460(12) 0.76829(17) 0.0375(5) Uani 1 1 d . . . C32 C 0.03628(8) 0.13698(14) 0.84239(19) 0.0488(6) Uani 1 1 d . . . H32A H 0.0133 0.1813 0.8355 0.059 Uiso 1 1 calc R . . H32B H 0.0362 0.1172 0.9102 0.059 Uiso 1 1 calc R . . C33 C 0.08471(8) 0.16617(15) 0.8123(2) 0.0585(7) Uani 1 1 d . . . H33A H 0.0906 0.2227 0.8343 0.070 Uiso 1 1 calc R . . H33B H 0.1090 0.1299 0.8386 0.070 Uiso 1 1 calc R . . C34 C 0.06244(7) 0.07963(13) 0.68359(18) 0.0436(6) Uani 1 1 d . . . H34 H 0.0466 0.0800 0.6190 0.052 Uiso 1 1 calc R . . C35 C 0.12567(9) 0.18135(17) 0.6549(2) 0.0763(9) Uani 1 1 d . . . H35A H 0.1349 0.2373 0.6710 0.114 Uiso 1 1 calc R . . H35B H 0.1211 0.1766 0.5847 0.114 Uiso 1 1 calc R . . H35C H 0.1499 0.1434 0.6757 0.114 Uiso 1 1 calc R . . C36 C 0.11898(10) -0.01934(17) 0.6007(2) 0.0784(9) Uani 1 1 d . . . H36A H 0.1517 -0.0284 0.6145 0.118 Uiso 1 1 calc R . . H36B H 0.1158 0.0216 0.5493 0.118 Uiso 1 1 calc R . . H36C H 0.1048 -0.0706 0.5795 0.118 Uiso 1 1 calc R . . N1 N 0.42414(7) 0.04657(12) 0.09549(15) 0.0509(5) Uani 1 1 d . . . N2 N 0.41976(7) -0.10682(12) 0.08674(17) 0.0541(6) Uani 1 1 d . . . N3 N 0.25229(7) -0.12825(12) -0.01865(16) 0.0538(6) Uani 1 1 d . . . N4 N 0.23850(7) 0.02265(13) -0.04157(16) 0.0591(6) Uani 1 1 d . . . N5 N 0.08206(7) 0.16122(11) 0.70548(17) 0.0520(6) Uani 1 1 d . . . N6 N 0.09574(6) 0.01008(11) 0.68988(16) 0.0520(6) 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 0.0384(14) 0.0515(15) 0.0422(16) -0.0040(12) 0.0040(12) 0.0042(11) C2 0.0528(16) 0.0570(17) 0.064(2) -0.0073(14) 0.0043(15) -0.0053(13) C3 0.068(2) 0.0568(18) 0.076(2) 0.0126(15) 0.0072(17) -0.0041(15) C4 0.0681(19) 0.074(2) 0.059(2) 0.0231(15) 0.0027(16) 0.0020(16) C5 0.0487(16) 0.0704(18) 0.0472(18) 0.0086(13) -0.0004(13) -0.0030(13) C6 0.0340(13) 0.0529(14) 0.0361(15) -0.0011(11) 0.0031(11) 0.0032(11) C7 0.0338(13) 0.0496(14) 0.0398(15) 0.0010(11) 0.0012(11) 0.0012(10) C8 0.0487(16) 0.0571(16) 0.0509(17) -0.0050(12) 0.0056(13) 0.0038(12) C9 0.0517(17) 0.0548(16) 0.075(2) -0.0039(14) 0.0072(15) 0.0088(12) C10 0.0329(13) 0.0591(16) 0.0459(16) 0.0049(12) 0.0013(11) 0.0033(12) C11 0.0489(17) 0.081(2) 0.103(3) 0.0169(17) -0.0159(17) 0.0129(15) C12 0.071(2) 0.089(2) 0.064(2) -0.0056(16) -0.0203(17) -0.0073(16) C13 0.0372(14) 0.0582(16) 0.0609(19) 0.0089(14) 0.0057(13) 0.0015(12) C14 0.0484(17) 0.0636(19) 0.105(3) 0.0186(18) 0.0121(17) 0.0085(15) C15 0.069(2) 0.0603(19) 0.118(3) -0.009(2) 0.028(2) 0.0024(17) C16 0.071(2) 0.083(2) 0.089(3) -0.0324(18) 0.021(2) -0.0057(18) C17 0.0499(16) 0.0765(19) 0.0556(19) -0.0125(15) 0.0095(14) 0.0014(14) C18 0.0336(13) 0.0565(15) 0.0448(16) 0.0017(12) 0.0061(12) -0.0017(11) C19 0.0329(13) 0.0524(14) 0.0394(15) 0.0022(11) 0.0016(11) -0.0010(11) C20 0.0472(15) 0.0624(17) 0.0506(17) 0.0086(13) 0.0038(13) -0.0001(12) C21 0.0495(16) 0.0590(16) 0.071(2) 0.0062(14) 0.0080(14) -0.0050(13) C22 0.0336(13) 0.0655(17) 0.0461(16) 0.0003(12) 0.0020(12) -0.0017(12) C23 0.0505(17) 0.085(2) 0.089(2) -0.0216(17) -0.0040(16) -0.0121(15) C24 0.071(2) 0.113(3) 0.079(2) 0.0260(19) -0.0293(19) 0.0050(18) C25 0.0394(14) 0.0421(14) 0.0499(17) -0.0059(11) -0.0006(12) 0.0011(11) C26 0.0478(16) 0.0488(15) 0.071(2) -0.0094(14) -0.0023(14) 0.0099(12) C27 0.0699(19) 0.0445(15) 0.070(2) -0.0001(14) -0.0100(16) 0.0145(14) C28 0.073(2) 0.0523(16) 0.0547(19) 0.0098(13) -0.0009(15) 0.0064(14) C29 0.0561(16) 0.0504(15) 0.0425(16) 0.0044(12) 0.0086(13) 0.0052(12) C30 0.0367(13) 0.0394(13) 0.0429(15) -0.0060(11) -0.0007(11) 0.0018(10) C31 0.0334(12) 0.0369(12) 0.0422(15) -0.0020(10) 0.0057(11) -0.0004(9) C32 0.0453(15) 0.0444(14) 0.0567(18) -0.0103(12) 0.0054(12) -0.0010(11) C33 0.0459(16) 0.0458(15) 0.084(2) -0.0141(13) 0.0016(15) -0.0069(11) C34 0.0329(13) 0.0453(14) 0.0526(16) -0.0016(11) 0.0077(12) -0.0021(11) C35 0.0544(18) 0.0682(19) 0.106(3) 0.0110(16) 0.0211(17) -0.0185(14) C36 0.074(2) 0.0686(19) 0.093(2) -0.0066(16) 0.0436(18) 0.0079(15) N1 0.0470(12) 0.0563(13) 0.0492(14) -0.0001(10) -0.0123(10) -0.0043(10) N2 0.0401(12) 0.0580(13) 0.0642(17) 0.0084(11) -0.0050(11) 0.0092(10) N3 0.0411(12) 0.0609(14) 0.0593(16) -0.0075(11) -0.0013(11) -0.0082(10) N4 0.0461(13) 0.0676(14) 0.0634(16) 0.0077(12) -0.0169(11) 0.0046(11) N5 0.0436(12) 0.0452(12) 0.0673(17) -0.0001(10) 0.0120(11) -0.0083(9) N6 0.0441(12) 0.0466(12) 0.0655(15) -0.0033(11) 0.0213(11) 0.0064(9) _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 N1 1.385(3) . ? C1 C2 1.386(3) . ? C1 C6 1.386(3) . ? C2 C3 1.383(4) . ? C2 H2 0.9300 . ? C3 C4 1.371(4) . ? C3 H3 0.9300 . ? C4 C5 1.385(3) . ? C4 H4 0.9300 . ? C5 C6 1.381(3) . ? C5 H5 0.9300 . ? C6 C7 1.513(3) . ? C7 C8 1.551(3) . ? C7 C19 1.561(3) . ? C7 C10 1.570(3) . ? C8 C9 1.509(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.448(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.454(3) . ? C10 N1 1.471(3) . ? C10 H10 0.9800 . ? C11 N2 1.452(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N1 1.443(3) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N4 1.386(3) . ? C13 C14 1.386(3) . ? C13 C18 1.389(3) . ? C14 C15 1.381(4) . ? C14 H14 0.9300 . ? C15 C16 1.363(4) . ? C15 H15 0.9300 . ? C16 C17 1.387(4) . ? C16 H16 0.9300 . ? C17 C18 1.373(3) . ? C17 H17 0.9300 . ? C18 C19 1.517(3) . ? C19 C20 1.550(3) . ? C19 C22 1.560(3) . ? C20 C21 1.501(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N3 1.451(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N3 1.456(3) . ? C22 N4 1.472(3) . ? C22 H22 0.9800 . ? C23 N3 1.449(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N4 1.445(3) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.384(3) . ? C25 N6 1.388(3) . ? C25 C30 1.390(3) . ? C26 C27 1.391(3) . ? C26 H26 0.9300 . ? C27 C28 1.369(3) . ? C27 H27 0.9300 . ? C28 C29 1.384(3) . ? C28 H28 0.9300 . ? C29 C30 1.377(3) . ? C29 H29 0.9300 . ? C30 C31 1.520(3) . ? C31 C31 1.558(4) 2_556 ? C31 C32 1.560(3) . ? C31 C34 1.566(3) . ? C32 C33 1.512(3) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 N5 1.447(3) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 N5 1.454(3) . ? C34 N6 1.467(3) . ? C34 H34 0.9800 . ? C35 N5 1.455(3) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 N6 1.456(3) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 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 N1 C1 C2 127.6(2) . . ? N1 C1 C6 111.3(2) . . ? C2 C1 C6 121.1(2) . . ? C3 C2 C1 118.6(2) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C4 C3 C2 120.8(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.4(3) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.7(2) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 119.4(2) . . ? C5 C6 C7 130.1(2) . . ? C1 C6 C7 110.5(2) . . ? C6 C7 C8 110.82(19) . . ? C6 C7 C19 113.91(17) . . ? C8 C7 C19 112.54(18) . . ? C6 C7 C10 102.22(17) . . ? C8 C7 C10 103.38(17) . . ? C19 C7 C10 113.04(18) . . ? C9 C8 C7 103.50(19) . . ? C9 C8 H8A 111.1 . . ? C7 C8 H8A 111.1 . . ? C9 C8 H8B 111.1 . . ? C7 C8 H8B 111.1 . . ? H8A C8 H8B 109.0 . . ? N2 C9 C8 102.1(2) . . ? N2 C9 H9A 111.3 . . ? C8 C9 H9A 111.3 . . ? N2 C9 H9B 111.3 . . ? C8 C9 H9B 111.3 . . ? H9A C9 H9B 109.2 . . ? N2 C10 N1 115.19(19) . . ? N2 C10 C7 104.33(18) . . ? N1 C10 C7 105.66(18) . . ? N2 C10 H10 110.4 . . ? N1 C10 H10 110.4 . . ? C7 C10 H10 110.4 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C14 128.0(3) . . ? N4 C13 C18 111.1(2) . . ? C14 C13 C18 120.9(3) . . ? C15 C14 C13 118.1(3) . . ? C15 C14 H14 121.0 . . ? C13 C14 H14 121.0 . . ? C16 C15 C14 121.7(3) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 119.8(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 119.6(2) . . ? C17 C18 C19 130.3(2) . . ? C13 C18 C19 110.2(2) . . ? C18 C19 C20 110.5(2) . . ? C18 C19 C22 102.72(18) . . ? C20 C19 C22 103.21(18) . . ? C18 C19 C7 113.42(18) . . ? C20 C19 C7 112.40(18) . . ? C22 C19 C7 113.76(18) . . ? C21 C20 C19 103.56(19) . . ? C21 C20 H20A 111.0 . . ? C19 C20 H20A 111.0 . . ? C21 C20 H20B 111.0 . . ? C19 C20 H20B 111.0 . . ? H20A C20 H20B 109.0 . . ? N3 C21 C20 102.04(19) . . ? N3 C21 H21A 111.4 . . ? C20 C21 H21A 111.4 . . ? N3 C21 H21B 111.4 . . ? C20 C21 H21B 111.4 . . ? H21A C21 H21B 109.2 . . ? N3 C22 N4 115.32(19) . . ? N3 C22 C19 104.82(19) . . ? N4 C22 C19 105.49(19) . . ? N3 C22 H22 110.3 . . ? N4 C22 H22 110.3 . . ? C19 C22 H22 110.3 . . ? N3 C23 H23A 109.5 . . ? N3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N6 127.2(2) . . ? C26 C25 C30 121.1(2) . . ? N6 C25 C30 111.7(2) . . ? C25 C26 C27 118.2(2) . . ? C25 C26 H26 120.9 . . ? C27 C26 H26 120.9 . . ? C28 C27 C26 120.9(2) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 120.6(2) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C30 C29 C28 119.5(2) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C25 119.8(2) . . ? C29 C30 C31 130.6(2) . . ? C25 C30 C31 109.58(19) . . ? C30 C31 C31 113.54(12) . 2_556 ? C30 C31 C32 110.67(18) . . ? C31 C31 C32 112.19(16) 2_556 . ? C30 C31 C34 102.71(16) . . ? C31 C31 C34 113.5(2) 2_556 . ? C32 C31 C34 103.38(17) . . ? C33 C32 C31 103.09(18) . . ? C33 C32 H32A 111.1 . . ? C31 C32 H32A 111.1 . . ? C33 C32 H32B 111.1 . . ? C31 C32 H32B 111.1 . . ? H32A C32 H32B 109.1 . . ? N5 C33 C32 102.0(2) . . ? N5 C33 H33A 111.4 . . ? C32 C33 H33A 111.4 . . ? N5 C33 H33B 111.4 . . ? C32 C33 H33B 111.4 . . ? H33A C33 H33B 109.2 . . ? N5 C34 N6 115.30(18) . . ? N5 C34 C31 104.19(17) . . ? N6 C34 C31 105.65(17) . . ? N5 C34 H34 110.5 . . ? N6 C34 H34 110.5 . . ? C31 C34 H34 110.5 . . ? N5 C35 H35A 109.5 . . ? N5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N6 C36 H36A 109.5 . . ? N6 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N6 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C1 N1 C12 120.7(2) . . ? C1 N1 C10 110.21(18) . . ? C12 N1 C10 121.0(2) . . ? C9 N2 C11 115.9(2) . . ? C9 N2 C10 106.25(18) . . ? C11 N2 C10 115.1(2) . . ? C23 N3 C21 114.8(2) . . ? C23 N3 C22 115.9(2) . . ? C21 N3 C22 105.75(19) . . ? C13 N4 C24 121.8(2) . . ? C13 N4 C22 110.53(19) . . ? C24 N4 C22 121.2(2) . . ? C33 N5 C34 105.68(18) . . ? C33 N5 C35 114.6(2) . . ? C34 N5 C35 115.6(2) . . ? C25 N6 C36 120.1(2) . . ? C25 N6 C34 110.16(18) . . ? C36 N6 C34 119.7(2) . . ? 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 176.7(2) . . . . ? C6 C1 C2 C3 -1.4(4) . . . . ? C1 C2 C3 C4 0.8(4) . . . . ? C2 C3 C4 C5 0.0(4) . . . . ? C3 C4 C5 C6 -0.3(4) . . . . ? C4 C5 C6 C1 -0.3(4) . . . . ? C4 C5 C6 C7 -178.6(2) . . . . ? N1 C1 C6 C5 -177.3(2) . . . . ? C2 C1 C6 C5 1.1(3) . . . . ? N1 C1 C6 C7 1.4(3) . . . . ? C2 C1 C6 C7 179.8(2) . . . . ? C5 C6 C7 C8 68.8(3) . . . . ? C1 C6 C7 C8 -109.7(2) . . . . ? C5 C6 C7 C19 -59.3(3) . . . . ? C1 C6 C7 C19 122.2(2) . . . . ? C5 C6 C7 C10 178.4(2) . . . . ? C1 C6 C7 C10 -0.1(2) . . . . ? C6 C7 C8 C9 89.8(2) . . . . ? C19 C7 C8 C9 -141.3(2) . . . . ? C10 C7 C8 C9 -19.0(2) . . . . ? C7 C8 C9 N2 39.4(2) . . . . ? C6 C7 C10 N2 -123.00(19) . . . . ? C8 C7 C10 N2 -7.8(2) . . . . ? C19 C7 C10 N2 114.1(2) . . . . ? C6 C7 C10 N1 -1.1(2) . . . . ? C8 C7 C10 N1 114.0(2) . . . . ? C19 C7 C10 N1 -124.00(19) . . . . ? N4 C13 C14 C15 178.1(3) . . . . ? C18 C13 C14 C15 -0.6(4) . . . . ? C13 C14 C15 C16 -0.5(4) . . . . ? C14 C15 C16 C17 0.8(5) . . . . ? C15 C16 C17 C18 -0.1(4) . . . . ? C16 C17 C18 C13 -0.9(4) . . . . ? C16 C17 C18 C19 -179.9(2) . . . . ? N4 C13 C18 C17 -177.7(2) . . . . ? C14 C13 C18 C17 1.2(4) . . . . ? N4 C13 C18 C19 1.5(3) . . . . ? C14 C13 C18 C19 -179.6(2) . . . . ? C17 C18 C19 C20 68.4(3) . . . . ? C13 C18 C19 C20 -110.7(2) . . . . ? C17 C18 C19 C22 178.0(2) . . . . ? C13 C18 C19 C22 -1.1(2) . . . . ? C17 C18 C19 C7 -58.8(3) . . . . ? C13 C18 C19 C7 122.1(2) . . . . ? C6 C7 C19 C18 -37.8(3) . . . . ? C8 C7 C19 C18 -165.01(19) . . . . ? C10 C7 C19 C18 78.3(2) . . . . ? C6 C7 C19 C20 -164.0(2) . . . . ? C8 C7 C19 C20 68.8(2) . . . . ? C10 C7 C19 C20 -47.9(3) . . . . ? C6 C7 C19 C22 79.1(2) . . . . ? C8 C7 C19 C22 -48.1(3) . . . . ? C10 C7 C19 C22 -164.76(18) . . . . ? C18 C19 C20 C21 89.1(2) . . . . ? C22 C19 C20 C21 -20.1(2) . . . . ? C7 C19 C20 C21 -143.1(2) . . . . ? C19 C20 C21 N3 40.2(2) . . . . ? C18 C19 C22 N3 -121.84(19) . . . . ? C20 C19 C22 N3 -6.9(2) . . . . ? C7 C19 C22 N3 115.2(2) . . . . ? C18 C19 C22 N4 0.3(2) . . . . ? C20 C19 C22 N4 115.3(2) . . . . ? C7 C19 C22 N4 -122.7(2) . . . . ? N6 C25 C26 C27 -179.7(2) . . . . ? C30 C25 C26 C27 0.7(4) . . . . ? C25 C26 C27 C28 -0.5(4) . . . . ? C26 C27 C28 C29 0.1(4) . . . . ? C27 C28 C29 C30 0.0(4) . . . . ? C28 C29 C30 C25 0.1(3) . . . . ? C28 C29 C30 C31 177.5(2) . . . . ? C26 C25 C30 C29 -0.5(3) . . . . ? N6 C25 C30 C29 179.8(2) . . . . ? C26 C25 C30 C31 -178.4(2) . . . . ? N6 C25 C30 C31 1.9(3) . . . . ? C29 C30 C31 C31 -53.6(4) . . . 2_556 ? C25 C30 C31 C31 124.0(2) . . . 2_556 ? C29 C30 C31 C32 73.6(3) . . . . ? C25 C30 C31 C32 -108.8(2) . . . . ? C29 C30 C31 C34 -176.6(2) . . . . ? C25 C30 C31 C34 1.0(2) . . . . ? C30 C31 C32 C33 91.7(2) . . . . ? C31 C31 C32 C33 -140.3(2) 2_556 . . . ? C34 C31 C32 C33 -17.6(2) . . . . ? C31 C32 C33 N5 39.4(2) . . . . ? C30 C31 C34 N5 -125.22(18) . . . . ? C31 C31 C34 N5 111.77(15) 2_556 . . . ? C32 C31 C34 N5 -10.0(2) . . . . ? C30 C31 C34 N6 -3.3(2) . . . . ? C31 C31 C34 N6 -126.31(14) 2_556 . . . ? C32 C31 C34 N6 111.88(19) . . . . ? C2 C1 N1 C12 30.6(4) . . . . ? C6 C1 N1 C12 -151.1(2) . . . . ? C2 C1 N1 C10 179.5(2) . . . . ? C6 C1 N1 C10 -2.2(3) . . . . ? N2 C10 N1 C1 116.6(2) . . . . ? C7 C10 N1 C1 2.0(2) . . . . ? N2 C10 N1 C12 -94.6(3) . . . . ? C7 C10 N1 C12 150.9(2) . . . . ? C8 C9 N2 C11 -175.7(2) . . . . ? C8 C9 N2 C10 -46.4(2) . . . . ? N1 C10 N2 C9 -81.7(2) . . . . ? C7 C10 N2 C9 33.6(2) . . . . ? N1 C10 N2 C11 48.0(3) . . . . ? C7 C10 N2 C11 163.3(2) . . . . ? C20 C21 N3 C23 -175.3(2) . . . . ? C20 C21 N3 C22 -46.3(2) . . . . ? N4 C22 N3 C23 45.8(3) . . . . ? C19 C22 N3 C23 161.3(2) . . . . ? N4 C22 N3 C21 -82.6(2) . . . . ? C19 C22 N3 C21 32.9(2) . . . . ? C14 C13 N4 C24 27.7(4) . . . . ? C18 C13 N4 C24 -153.5(2) . . . . ? C14 C13 N4 C22 179.9(3) . . . . ? C18 C13 N4 C22 -1.3(3) . . . . ? N3 C22 N4 C13 115.7(2) . . . . ? C19 C22 N4 C13 0.5(3) . . . . ? N3 C22 N4 C24 -91.9(3) . . . . ? C19 C22 N4 C24 152.9(2) . . . . ? C32 C33 N5 C34 -48.0(2) . . . . ? C32 C33 N5 C35 -176.43(19) . . . . ? N6 C34 N5 C33 -79.3(2) . . . . ? C31 C34 N5 C33 36.0(2) . . . . ? N6 C34 N5 C35 48.5(3) . . . . ? C31 C34 N5 C35 163.8(2) . . . . ? C26 C25 N6 C36 30.7(4) . . . . ? C30 C25 N6 C36 -149.6(2) . . . . ? C26 C25 N6 C34 176.1(2) . . . . ? C30 C25 N6 C34 -4.3(3) . . . . ? N5 C34 N6 C25 119.1(2) . . . . ? C31 C34 N6 C25 4.7(2) . . . . ? N5 C34 N6 C36 -95.4(3) . . . . ? C31 C34 N6 C36 150.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.159 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.037