data_s92 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H48 N8' _chemical_formula_weight 640.86 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 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 8.71760(10) _cell_length_b 13.4265(2) _cell_length_c 16.1511(4) _cell_angle_alpha 95.5550(10) _cell_angle_beta 101.9900(10) _cell_angle_gamma 104.5180(10) _cell_volume 1767.88(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7201 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour yellow _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 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9784 _exptl_absorpt_correction_T_max 0.9891 _exptl_absorpt_process_details 'SORTAV (R.H. Blessing, 1995, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method '\w and \f scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number 'n/a' _diffrn_standards_interval_count 'n/a' _diffrn_standards_interval_time 'n/a' _diffrn_standards_decay_% 'n/a' _diffrn_reflns_number 17542 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6236 _reflns_number_gt 4400 _reflns_threshold_expression >2\s(I) _computing_data_collection ; 'DENZO (Otwinowski and Minor, 1997) & COLLECT (Hooft, 1998) ' ; _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material SHELXL-97 _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^ > 2\s(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^)+(0.0551P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0144(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6236 _refine_ls_number_parameters 626 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 N8 N 0.16261(15) 0.75243(10) 0.03030(8) 0.0259(3) Uani 1 1 d . . . N7 N 0.31657(15) 0.68409(9) -0.05034(8) 0.0250(3) Uani 1 1 d . . . C30 C 0.24357(18) 0.75721(11) -0.03120(9) 0.0246(4) Uani 1 1 d . . . C28 C 0.22472(18) 0.82607(12) -0.16942(9) 0.0246(4) Uani 1 1 d . . . C26 C 0.29857(18) 0.94731(12) -0.03889(10) 0.0256(4) Uani 1 1 d . . . C29 C 0.23968(18) 0.90726(12) -0.21556(10) 0.0240(4) Uani 1 1 d . . . C24 C 0.28625(17) 1.01142(11) -0.17514(9) 0.0236(4) Uani 1 1 d . . . C25 C 0.31485(18) 1.02833(12) -0.08509(10) 0.0252(4) Uani 1 1 d . . . N6 N 0.38631(19) 1.28298(11) -0.14135(9) 0.0431(4) Uani 1 1 d . . . C23 C 0.30523(19) 1.09685(12) -0.22290(9) 0.0271(4) Uani 1 1 d . . . C22 C 0.3497(2) 1.19988(13) -0.18025(10) 0.0302(4) Uani 1 1 d . . . C21 C 0.2890(2) 1.08022(12) -0.31234(11) 0.0309(4) Uani 1 1 d . . . C27 C 0.25446(18) 0.84408(11) -0.07996(9) 0.0235(3) Uani 1 1 d . . . C36 C 0.0224(2) 0.79623(14) 0.02762(11) 0.0312(4) Uani 1 1 d . . . N5 N 0.2750(2) 1.06509(11) -0.38559(10) 0.0452(4) Uani 1 1 d . . . C31 C 0.46728(19) 0.70805(13) -0.08164(10) 0.0281(4) Uani 1 1 d . . . C33 C 0.3945(2) 0.52446(14) -0.15461(12) 0.0368(4) Uani 1 1 d . . . C32 C 0.4503(2) 0.63816(13) -0.16440(11) 0.0326(4) Uani 1 1 d . . . C35 C 0.2622(2) 0.57463(12) -0.03765(11) 0.0317(4) Uani 1 1 d . . . C40 C 0.1971(2) 0.69953(15) 0.10497(11) 0.0357(4) Uani 1 1 d . . . C34 C 0.2423(2) 0.50291(14) -0.12047(12) 0.0358(4) Uani 1 1 d . . . C39 C 0.2243(3) 0.77432(18) 0.18655(11) 0.0442(5) Uani 1 1 d . . . C37 C 0.0461(2) 0.87091(15) 0.10902(11) 0.0360(4) Uani 1 1 d . . . C38 C 0.0803(2) 0.81871(17) 0.18756(12) 0.0402(5) Uani 1 1 d . . . N4 N 0.86631(15) 0.74492(10) 0.48592(7) 0.0255(3) Uani 1 1 d . . . N3 N 0.70826(14) 0.80855(10) 0.56665(7) 0.0256(3) Uani 1 1 d . . . C10 C 0.72090(18) 0.74530(11) 0.50014(9) 0.0242(4) Uani 1 1 d . . . C6 C 0.54930(19) 0.65864(12) 0.35474(10) 0.0262(4) Uani 1 1 d . . . C8 C 0.45102(19) 0.61632(12) 0.47887(10) 0.0264(4) Uani 1 1 d . . . C7 C 0.57236(18) 0.67381(11) 0.44423(9) 0.0248(4) Uani 1 1 d . . . C9 C 0.31376(19) 0.54513(12) 0.42707(10) 0.0275(4) Uani 1 1 d . . . C5 C 0.41207(19) 0.58821(12) 0.30311(10) 0.0279(4) Uani 1 1 d . . . C4 C 0.29097(18) 0.52846(12) 0.33731(10) 0.0274(4) Uani 1 1 d . . . C2 C 0.14939(19) 0.45279(12) 0.28330(10) 0.0305(4) Uani 1 1 d . . . C19 C 1.0986(2) 0.85889(14) 0.44480(11) 0.0339(4) Uani 1 1 d . . . C17 C 0.9821(2) 0.67557(14) 0.37228(10) 0.0330(4) Uani 1 1 d . . . C11 C 0.5740(2) 0.85806(14) 0.55974(11) 0.0307(4) Uani 1 1 d . . . C16 C 0.8981(2) 0.65133(13) 0.44416(10) 0.0285(4) Uani 1 1 d . . . C20 C 1.01223(19) 0.83532(13) 0.51598(11) 0.0299(4) Uani 1 1 d . . . C15 C 0.8315(2) 0.84111(15) 0.64897(10) 0.0326(4) Uani 1 1 d . . . N2 N 0.12560(18) 0.41194(12) 0.12157(10) 0.0474(4) Uani 1 1 d . . . N1 N -0.0799(2) 0.35758(13) 0.34852(10) 0.0506(4) Uani 1 1 d . . . C12 C 0.4905(2) 0.84347(15) 0.63316(11) 0.0371(4) Uani 1 1 d . . . C18 C 1.1382(2) 0.76353(14) 0.40598(11) 0.0349(4) Uani 1 1 d . . . C1 C 0.0234(2) 0.39983(13) 0.31800(11) 0.0356(4) Uani 1 1 d . . . C3 C 0.13392(19) 0.42923(13) 0.19432(11) 0.0344(4) Uani 1 1 d . . . C13 C 0.6149(2) 0.87770(17) 0.71921(12) 0.0432(5) Uani 1 1 d . . . C14 C 0.7475(2) 0.82243(17) 0.72214(12) 0.0414(5) Uani 1 1 d . . . H5 H 0.4000(19) 0.5780(12) 0.2387(11) 0.036(4) Uiso 1 1 d . . . H35A H 0.1570(19) 0.5632(11) -0.0208(9) 0.025(4) Uiso 1 1 d . . . H28 H 0.1930(17) 0.7537(12) -0.1987(9) 0.026(4) Uiso 1 1 d . . . H31B H 0.4962(19) 0.7828(13) -0.0882(10) 0.031(4) Uiso 1 1 d . . . H31A H 0.5516(19) 0.6954(11) -0.0352(10) 0.027(4) Uiso 1 1 d . . . H8 H 0.4694(19) 0.6248(12) 0.5421(10) 0.030(4) Uiso 1 1 d . . . H20B H 0.9773(19) 0.8973(13) 0.5358(10) 0.037(4) Uiso 1 1 d . . . H29 H 0.2185(17) 0.8925(11) -0.2785(9) 0.021(4) Uiso 1 1 d . . . H20A H 1.0916(19) 0.8196(11) 0.5648(10) 0.027(4) Uiso 1 1 d . . . H25 H 0.3505(17) 1.1010(12) -0.0535(9) 0.024(4) Uiso 1 1 d . . . H36A H 0.0066(18) 0.8272(12) -0.0274(10) 0.031(4) Uiso 1 1 d . . . H40A H 0.297(2) 0.6810(13) 0.1036(10) 0.040(5) Uiso 1 1 d . . . H26 H 0.3234(18) 0.9617(11) 0.0244(10) 0.028(4) Uiso 1 1 d . . . H16A H 0.9684(17) 0.6290(11) 0.4898(9) 0.019(4) Uiso 1 1 d . . . H19A H 1.032(2) 0.8841(12) 0.4001(10) 0.035(4) Uiso 1 1 d . . . H19B H 1.202(2) 0.9188(13) 0.4721(10) 0.034(4) Uiso 1 1 d . . . H16B H 0.7922(19) 0.5960(12) 0.4249(9) 0.024(4) Uiso 1 1 d . . . H6 H 0.6349(18) 0.7016(11) 0.3279(9) 0.023(4) Uiso 1 1 d . . . H9 H 0.2282(19) 0.5034(12) 0.4518(9) 0.027(4) Uiso 1 1 d . . . H17A H 0.9078(19) 0.6965(12) 0.3252(10) 0.031(4) Uiso 1 1 d . . . H12A H 0.427(2) 0.7698(14) 0.6273(10) 0.034(4) Uiso 1 1 d . . . H18B H 1.194(2) 0.7774(13) 0.3597(11) 0.044(5) Uiso 1 1 d . . . H14A H 0.834(2) 0.8483(13) 0.7754(11) 0.043(5) Uiso 1 1 d . . . H15A H 0.890(2) 0.9139(14) 0.6547(10) 0.034(5) Uiso 1 1 d . . . H11B H 0.622(2) 0.9348(14) 0.5616(10) 0.038(5) Uiso 1 1 d . . . H18A H 1.213(2) 0.7404(13) 0.4504(11) 0.040(5) Uiso 1 1 d . . . H32A H 0.557(2) 0.6516(13) -0.1803(10) 0.041(5) Uiso 1 1 d . . . H32B H 0.370(2) 0.6536(12) -0.2135(11) 0.037(4) Uiso 1 1 d . . . H34A H 0.150(2) 0.5095(13) -0.1659(11) 0.046(5) Uiso 1 1 d . . . H33A H 0.484(2) 0.5098(13) -0.1162(10) 0.037(5) Uiso 1 1 d . . . H15B H 0.911(2) 0.7986(12) 0.6468(10) 0.035(4) Uiso 1 1 d . . . H35B H 0.350(2) 0.5625(12) 0.0111(10) 0.035(4) Uiso 1 1 d . . . H11A H 0.496(2) 0.8307(12) 0.5030(11) 0.036(4) Uiso 1 1 d . . . H36B H -0.076(2) 0.7349(14) 0.0218(10) 0.041(5) Uiso 1 1 d . . . H38A H -0.024(2) 0.7606(14) 0.1836(11) 0.046(5) Uiso 1 1 d . . . H33B H 0.373(2) 0.4784(14) -0.2119(11) 0.044(5) Uiso 1 1 d . . . H37A H -0.056(2) 0.8938(13) 0.1050(11) 0.045(5) Uiso 1 1 d . . . H13B H 0.560(2) 0.8626(13) 0.7654(12) 0.047(5) Uiso 1 1 d . . . H17B H 1.0051(19) 0.6096(13) 0.3484(10) 0.039(5) Uiso 1 1 d . . . H13A H 0.666(2) 0.9561(16) 0.7257(12) 0.054(6) Uiso 1 1 d . . . H37B H 0.139(2) 0.9343(15) 0.1107(11) 0.053(6) Uiso 1 1 d . . . H12B H 0.413(2) 0.8884(13) 0.6295(10) 0.036(4) Uiso 1 1 d . . . H34B H 0.213(2) 0.4285(14) -0.1087(10) 0.044(5) Uiso 1 1 d . . . H14B H 0.697(2) 0.7448(15) 0.7162(11) 0.044(5) Uiso 1 1 d . . . H39A H 0.248(2) 0.7392(14) 0.2350(12) 0.053(5) Uiso 1 1 d . . . H40B H 0.098(2) 0.6376(15) 0.0991(11) 0.047(5) Uiso 1 1 d . . . H39B H 0.323(3) 0.8320(16) 0.1929(12) 0.060(7) Uiso 1 1 d . . . H38B H 0.099(2) 0.8685(15) 0.2411(12) 0.056(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N8 0.0276(7) 0.0294(7) 0.0251(7) 0.0064(6) 0.0095(6) 0.0124(6) N7 0.0298(7) 0.0232(7) 0.0254(7) 0.0060(5) 0.0104(6) 0.0098(6) C30 0.0250(8) 0.0251(9) 0.0220(8) 0.0017(6) 0.0022(7) 0.0077(7) C28 0.0263(9) 0.0226(9) 0.0248(9) 0.0010(7) 0.0053(7) 0.0082(7) C26 0.0270(9) 0.0297(9) 0.0208(9) 0.0029(7) 0.0051(7) 0.0099(7) C29 0.0244(9) 0.0275(9) 0.0207(8) 0.0027(7) 0.0048(7) 0.0092(7) C24 0.0199(8) 0.0254(9) 0.0264(8) 0.0037(7) 0.0047(6) 0.0086(7) C25 0.0268(9) 0.0205(9) 0.0272(9) 0.0005(7) 0.0046(7) 0.0075(7) N6 0.0599(10) 0.0282(9) 0.0409(9) 0.0069(7) 0.0112(7) 0.0121(8) C23 0.0324(9) 0.0232(9) 0.0263(9) 0.0052(7) 0.0068(7) 0.0087(7) C22 0.0353(10) 0.0279(10) 0.0300(9) 0.0098(8) 0.0091(7) 0.0104(8) C21 0.0359(10) 0.0233(9) 0.0341(10) 0.0078(7) 0.0078(8) 0.0085(7) C27 0.0237(8) 0.0238(8) 0.0235(8) 0.0036(6) 0.0054(6) 0.0079(7) C36 0.0280(10) 0.0378(10) 0.0336(10) 0.0080(8) 0.0106(8) 0.0161(9) N5 0.0691(11) 0.0312(9) 0.0340(9) 0.0074(7) 0.0116(8) 0.0117(8) C31 0.0266(9) 0.0291(10) 0.0321(9) 0.0089(7) 0.0113(7) 0.0090(8) C33 0.0441(11) 0.0330(10) 0.0402(11) 0.0043(8) 0.0169(9) 0.0179(9) C32 0.0363(10) 0.0358(10) 0.0334(10) 0.0073(8) 0.0161(8) 0.0169(8) C35 0.0369(10) 0.0256(9) 0.0385(10) 0.0103(7) 0.0159(8) 0.0117(8) C40 0.0443(11) 0.0445(11) 0.0313(10) 0.0159(8) 0.0180(8) 0.0245(10) C34 0.0415(11) 0.0233(10) 0.0461(11) 0.0028(8) 0.0171(9) 0.0106(8) C39 0.0577(14) 0.0642(14) 0.0256(10) 0.0125(9) 0.0150(9) 0.0374(13) C37 0.0374(11) 0.0410(11) 0.0373(10) 0.0061(8) 0.0152(8) 0.0197(10) C38 0.0470(12) 0.0482(12) 0.0343(11) 0.0077(9) 0.0192(9) 0.0213(10) N4 0.0238(7) 0.0286(7) 0.0237(7) 0.0024(6) 0.0075(5) 0.0056(6) N3 0.0243(7) 0.0290(7) 0.0227(7) 0.0004(6) 0.0068(5) 0.0062(6) C10 0.0257(9) 0.0260(9) 0.0220(8) 0.0057(7) 0.0074(7) 0.0070(7) C6 0.0260(9) 0.0288(9) 0.0260(9) 0.0062(7) 0.0081(7) 0.0093(8) C8 0.0279(9) 0.0274(9) 0.0233(9) 0.0045(7) 0.0048(7) 0.0076(7) C7 0.0251(8) 0.0251(8) 0.0246(8) 0.0031(7) 0.0059(7) 0.0080(7) C9 0.0257(9) 0.0261(9) 0.0298(9) 0.0064(7) 0.0074(7) 0.0041(7) C5 0.0272(9) 0.0323(9) 0.0263(9) 0.0032(7) 0.0050(7) 0.0135(8) C4 0.0270(9) 0.0260(9) 0.0283(9) 0.0021(7) 0.0016(7) 0.0110(7) C2 0.0297(9) 0.0273(9) 0.0302(9) 0.0011(7) 0.0023(7) 0.0056(8) C19 0.0311(10) 0.0373(10) 0.0332(10) 0.0072(8) 0.0129(8) 0.0047(9) C17 0.0347(10) 0.0418(11) 0.0267(9) 0.0032(8) 0.0093(8) 0.0171(9) C11 0.0283(9) 0.0288(10) 0.0360(10) 0.0021(8) 0.0090(8) 0.0100(8) C16 0.0296(10) 0.0286(9) 0.0275(9) 0.0024(7) 0.0051(8) 0.0106(8) C20 0.0247(9) 0.0306(10) 0.0308(9) -0.0005(7) 0.0089(7) 0.0012(8) C15 0.0283(9) 0.0405(11) 0.0254(9) -0.0016(8) 0.0048(7) 0.0068(9) N2 0.0419(9) 0.0530(10) 0.0383(10) -0.0087(8) 0.0019(7) 0.0095(8) N1 0.0470(10) 0.0513(10) 0.0340(9) 0.0045(8) -0.0025(8) -0.0102(9) C12 0.0337(10) 0.0378(11) 0.0436(11) 0.0022(8) 0.0170(8) 0.0120(9) C18 0.0311(10) 0.0482(11) 0.0300(10) 0.0071(8) 0.0138(8) 0.0137(9) C1 0.0367(11) 0.0300(10) 0.0282(10) -0.0004(8) -0.0063(8) 0.0016(9) C3 0.0271(9) 0.0330(10) 0.0360(11) -0.0032(8) -0.0010(8) 0.0062(8) C13 0.0424(11) 0.0534(14) 0.0367(11) -0.0006(9) 0.0203(9) 0.0123(10) C14 0.0394(11) 0.0585(14) 0.0264(10) 0.0023(9) 0.0110(8) 0.0129(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N8 C30 1.3304(19) . ? N8 C40 1.474(2) . ? N8 C36 1.4783(18) . ? N7 C30 1.3419(17) . ? N7 C35 1.475(2) . ? N7 C31 1.477(2) . ? C30 C27 1.464(2) . ? C28 C29 1.374(2) . ? C28 C27 1.399(2) . ? C28 H28 0.983(15) . ? C26 C25 1.373(2) . ? C26 C27 1.399(2) . ? C26 H26 0.989(15) . ? C29 C24 1.405(2) . ? C29 H29 0.985(14) . ? C24 C25 1.409(2) . ? C24 C23 1.438(2) . ? C25 H25 0.997(15) . ? N6 C22 1.159(2) . ? C23 C22 1.405(2) . ? C23 C21 1.412(2) . ? C21 N5 1.156(2) . ? C36 C37 1.518(2) . ? C36 H36A 1.016(16) . ? C36 H36B 1.008(19) . ? C31 C32 1.515(2) . ? C31 H31B 0.994(17) . ? C31 H31A 0.995(15) . ? C33 C34 1.514(2) . ? C33 C32 1.516(2) . ? C33 H33A 0.966(16) . ? C33 H33B 1.017(17) . ? C32 H32A 0.996(18) . ? C32 H32B 1.017(16) . ? C35 C34 1.522(2) . ? C35 H35A 0.990(15) . ? C35 H35B 1.034(16) . ? C40 C39 1.515(2) . ? C40 H40A 0.970(17) . ? C40 H40B 1.02(2) . ? C34 H34A 0.999(17) . ? C34 H34B 1.013(18) . ? C39 C38 1.521(2) . ? C39 H39A 0.96(2) . ? C39 H39B 0.98(2) . ? C37 C38 1.520(2) . ? C37 H37A 1.005(17) . ? C37 H37B 1.01(2) . ? C38 H38A 1.023(19) . ? C38 H38B 0.997(19) . ? N4 C10 1.3355(19) . ? N4 C20 1.477(2) . ? N4 C16 1.4830(18) . ? N3 C10 1.3443(18) . ? N3 C15 1.473(2) . ? N3 C11 1.4745(18) . ? C10 C7 1.462(2) . ? C6 C5 1.374(2) . ? C6 C7 1.405(2) . ? C6 H6 1.022(16) . ? C8 C9 1.379(2) . ? C8 C7 1.396(2) . ? C8 H8 0.992(16) . ? C9 C4 1.409(2) . ? C9 H9 0.993(17) . ? C5 C4 1.402(2) . ? C5 H5 1.015(16) . ? C4 C2 1.438(2) . ? C2 C1 1.403(3) . ? C2 C3 1.412(2) . ? C19 C20 1.516(2) . ? C19 C18 1.519(2) . ? C19 H19A 0.972(16) . ? C19 H19B 1.028(17) . ? C17 C16 1.515(2) . ? C17 C18 1.518(3) . ? C17 H17A 1.002(16) . ? C17 H17B 1.014(16) . ? C11 C12 1.519(2) . ? C11 H11B 1.006(18) . ? C11 H11A 0.993(17) . ? C16 H16A 0.977(14) . ? C16 H16B 0.997(16) . ? C20 H20B 1.002(16) . ? C20 H20A 1.011(15) . ? C15 C14 1.523(2) . ? C15 H15A 0.967(18) . ? C15 H15B 1.009(16) . ? N2 C3 1.159(2) . ? N1 C1 1.165(2) . ? C12 C13 1.523(3) . ? C12 H12A 0.988(18) . ? C12 H12B 1.013(16) . ? C18 H18B 0.982(19) . ? C18 H18A 0.992(17) . ? C13 C14 1.517(2) . ? C13 H13B 0.979(19) . ? C13 H13A 1.02(2) . ? C14 H14A 0.987(18) . ? C14 H14B 1.011(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 N8 C40 124.16(12) . . ? C30 N8 C36 122.45(13) . . ? C40 N8 C36 113.33(13) . . ? C30 N7 C35 124.23(13) . . ? C30 N7 C31 122.39(13) . . ? C35 N7 C31 113.29(12) . . ? N8 C30 N7 121.80(13) . . ? N8 C30 C27 119.82(12) . . ? N7 C30 C27 118.38(13) . . ? C29 C28 C27 121.07(14) . . ? C29 C28 H28 120.5(9) . . ? C27 C28 H28 118.4(9) . . ? C25 C26 C27 120.80(14) . . ? C25 C26 H26 120.0(9) . . ? C27 C26 H26 119.2(9) . . ? C28 C29 C24 121.59(14) . . ? C28 C29 H29 119.5(8) . . ? C24 C29 H29 118.9(8) . . ? C29 C24 C25 116.71(14) . . ? C29 C24 C23 121.89(13) . . ? C25 C24 C23 121.40(13) . . ? C26 C25 C24 121.82(14) . . ? C26 C25 H25 118.6(8) . . ? C24 C25 H25 119.6(8) . . ? C22 C23 C21 118.38(14) . . ? C22 C23 C24 120.19(13) . . ? C21 C23 C24 121.33(13) . . ? N6 C22 C23 176.66(17) . . ? N5 C21 C23 179.02(18) . . ? C26 C27 C28 118.01(14) . . ? C26 C27 C30 121.36(13) . . ? C28 C27 C30 120.62(13) . . ? N8 C36 C37 111.48(13) . . ? N8 C36 H36A 106.4(8) . . ? C37 C36 H36A 115.3(8) . . ? N8 C36 H36B 105.9(9) . . ? C37 C36 H36B 109.8(9) . . ? H36A C36 H36B 107.6(13) . . ? N7 C31 C32 112.21(14) . . ? N7 C31 H31B 108.5(9) . . ? C32 C31 H31B 111.6(9) . . ? N7 C31 H31A 104.5(9) . . ? C32 C31 H31A 109.9(8) . . ? H31B C31 H31A 109.9(12) . . ? C34 C33 C32 110.84(13) . . ? C34 C33 H33A 111.5(10) . . ? C32 C33 H33A 106.9(10) . . ? C34 C33 H33B 110.1(10) . . ? C32 C33 H33B 110.0(10) . . ? H33A C33 H33B 107.3(13) . . ? C31 C32 C33 110.61(15) . . ? C31 C32 H32A 109.9(9) . . ? C33 C32 H32A 108.8(10) . . ? C31 C32 H32B 110.9(9) . . ? C33 C32 H32B 109.8(9) . . ? H32A C32 H32B 106.7(13) . . ? N7 C35 C34 109.50(14) . . ? N7 C35 H35A 108.7(8) . . ? C34 C35 H35A 110.3(8) . . ? N7 C35 H35B 107.6(9) . . ? C34 C35 H35B 110.8(8) . . ? H35A C35 H35B 109.8(12) . . ? N8 C40 C39 109.49(14) . . ? N8 C40 H40A 106.1(10) . . ? C39 C40 H40A 109.1(10) . . ? N8 C40 H40B 107.0(10) . . ? C39 C40 H40B 110.6(10) . . ? H40A C40 H40B 114.2(14) . . ? C33 C34 C35 112.89(15) . . ? C33 C34 H34A 108.3(10) . . ? C35 C34 H34A 110.8(9) . . ? C33 C34 H34B 109.8(10) . . ? C35 C34 H34B 107.8(10) . . ? H34A C34 H34B 107.2(14) . . ? C40 C39 C38 112.15(16) . . ? C40 C39 H39A 108.8(11) . . ? C38 C39 H39A 111.7(11) . . ? C40 C39 H39B 109.9(12) . . ? C38 C39 H39B 108.8(11) . . ? H39A C39 H39B 105.2(16) . . ? C36 C37 C38 110.78(15) . . ? C36 C37 H37A 107.5(10) . . ? C38 C37 H37A 110.9(10) . . ? C36 C37 H37B 108.1(10) . . ? C38 C37 H37B 111.4(10) . . ? H37A C37 H37B 108.0(14) . . ? C37 C38 C39 109.68(15) . . ? C37 C38 H38A 106.0(10) . . ? C39 C38 H38A 110.9(9) . . ? C37 C38 H38B 110.7(11) . . ? C39 C38 H38B 111.9(10) . . ? H38A C38 H38B 107.5(15) . . ? C10 N4 C20 122.88(13) . . ? C10 N4 C16 122.88(13) . . ? C20 N4 C16 114.10(12) . . ? C10 N3 C15 123.76(12) . . ? C10 N3 C11 121.64(12) . . ? C15 N3 C11 114.42(12) . . ? N4 C10 N3 121.18(13) . . ? N4 C10 C7 119.85(13) . . ? N3 C10 C7 118.95(13) . . ? C5 C6 C7 120.77(16) . . ? C5 C6 H6 119.8(8) . . ? C7 C6 H6 119.4(8) . . ? C9 C8 C7 121.14(15) . . ? C9 C8 H8 120.7(9) . . ? C7 C8 H8 118.1(9) . . ? C8 C7 C6 118.08(14) . . ? C8 C7 C10 120.55(13) . . ? C6 C7 C10 121.34(14) . . ? C8 C9 C4 121.06(16) . . ? C8 C9 H9 121.2(9) . . ? C4 C9 H9 117.8(9) . . ? C6 C5 C4 121.63(15) . . ? C6 C5 H5 118.9(10) . . ? C4 C5 H5 119.4(10) . . ? C5 C4 C9 117.30(14) . . ? C5 C4 C2 121.56(14) . . ? C9 C4 C2 121.14(15) . . ? C1 C2 C3 118.25(14) . . ? C1 C2 C4 120.67(14) . . ? C3 C2 C4 121.08(16) . . ? C20 C19 C18 111.58(15) . . ? C20 C19 H19A 110.4(10) . . ? C18 C19 H19A 109.4(9) . . ? C20 C19 H19B 105.9(9) . . ? C18 C19 H19B 112.0(8) . . ? H19A C19 H19B 107.4(13) . . ? C16 C17 C18 109.86(14) . . ? C16 C17 H17A 109.8(9) . . ? C18 C17 H17A 109.5(9) . . ? C16 C17 H17B 107.9(10) . . ? C18 C17 H17B 111.5(9) . . ? H17A C17 H17B 108.3(12) . . ? N3 C11 C12 112.20(13) . . ? N3 C11 H11B 107.5(9) . . ? C12 C11 H11B 108.4(9) . . ? N3 C11 H11A 109.0(9) . . ? C12 C11 H11A 112.0(10) . . ? H11B C11 H11A 107.6(13) . . ? N4 C16 C17 111.81(14) . . ? N4 C16 H16A 105.1(8) . . ? C17 C16 H16A 110.6(8) . . ? N4 C16 H16B 107.7(8) . . ? C17 C16 H16B 113.2(8) . . ? H16A C16 H16B 108.1(12) . . ? N4 C20 C19 110.98(13) . . ? N4 C20 H20B 108.7(9) . . ? C19 C20 H20B 109.5(10) . . ? N4 C20 H20A 109.6(9) . . ? C19 C20 H20A 108.0(9) . . ? H20B C20 H20A 110.1(12) . . ? N3 C15 C14 109.36(15) . . ? N3 C15 H15A 109.9(9) . . ? C14 C15 H15A 110.5(9) . . ? N3 C15 H15B 106.4(9) . . ? C14 C15 H15B 112.2(9) . . ? H15A C15 H15B 108.4(13) . . ? C11 C12 C13 110.83(16) . . ? C11 C12 H12A 109.7(9) . . ? C13 C12 H12A 110.8(9) . . ? C11 C12 H12B 107.8(9) . . ? C13 C12 H12B 108.8(9) . . ? H12A C12 H12B 108.8(13) . . ? C17 C18 C19 109.56(14) . . ? C17 C18 H18B 109.6(10) . . ? C19 C18 H18B 112.6(10) . . ? C17 C18 H18A 108.5(10) . . ? C19 C18 H18A 109.8(9) . . ? H18B C18 H18A 106.5(14) . . ? N1 C1 C2 178.41(18) . . ? N2 C3 C2 178.01(19) . . ? C14 C13 C12 110.26(15) . . ? C14 C13 H13B 110.5(10) . . ? C12 C13 H13B 109.5(11) . . ? C14 C13 H13A 109.0(10) . . ? C12 C13 H13A 108.0(10) . . ? H13B C13 H13A 109.6(14) . . ? C13 C14 C15 111.79(16) . . ? C13 C14 H14A 111.3(9) . . ? C15 C14 H14A 106.0(10) . . ? C13 C14 H14B 109.2(10) . . ? C15 C14 H14B 107.4(10) . . ? H14A C14 H14B 111.0(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.163 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.038