# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Lin Li' _publ_contact_author_email 'AHU LINLI@163.COM' _publ_section_title ; Two-photon Absorption Enhancement Induced by Aggregation with Accurate Photonphysical Data: Spontaneous Accumulation of Dye in Silica Nanoparticles ; loop_ _publ_author_name 'Lin Li.' 'Minhua Jiang.' 'Baokang Jin.' 'Lin Kong.' 'Pingping Sun.' ; Xukang Tao ; 'Yupeng Tian.' 'Jieying Wu.' 'Jiaxiang Yang.' 'Shengyi Zhang.' ; Hongping Zhou ; # Attachment 'crystal-data.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 752289' #TrackingRef 'crystal-data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H74 N8 O3' _chemical_formula_weight 931.25 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2690(14) _cell_length_b 12.2153(15) _cell_length_c 37.978(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.248(2) _cell_angle_gamma 90.00 _cell_volume 5223.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1639 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 19.72 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9890 _exptl_absorpt_correction_T_max 0.9912 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36465 _diffrn_reflns_av_R_equivalents 0.1073 _diffrn_reflns_av_sigmaI/netI 0.1199 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9216 _reflns_number_gt 4380 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SIR97 (Altamore, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'WINGX (Farrugia,1999)' _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^)+(0.1105P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0074(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9216 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1665 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.2424 _refine_ls_wR_factor_gt 0.1857 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.2474(3) 0.6666(3) 0.31075(10) 0.0317(9) Uani 1 1 d . . . C2 C 1.1429(3) 0.7776(3) 0.34765(10) 0.0307(9) Uani 1 1 d . . . C3 C 1.1354(3) 0.8431(3) 0.37944(10) 0.0362(10) Uani 1 1 d . . . H3 H 1.0665 0.8840 0.3817 0.043 Uiso 1 1 calc R . . C4 C 1.2177(4) 0.8506(3) 0.40577(10) 0.0368(10) Uani 1 1 d . . . H4 H 1.2864 0.8091 0.4039 0.044 Uiso 1 1 calc R . . C5 C 1.2086(4) 0.9183(3) 0.43721(11) 0.0380(10) Uani 1 1 d . . . C6 C 1.2870(4) 0.9083(3) 0.46591(11) 0.0416(11) Uani 1 1 d . . . H6 H 1.3480 0.8571 0.4651 0.050 Uiso 1 1 calc R . . C7 C 1.2777(4) 0.9716(3) 0.49569(11) 0.0482(12) Uani 1 1 d . . . H7 H 1.3329 0.9622 0.5143 0.058 Uiso 1 1 calc R . . C8 C 1.1880(4) 1.0494(4) 0.49884(12) 0.0525(13) Uani 1 1 d . . . C9 C 1.1095(5) 1.0598(5) 0.46925(14) 0.0802(18) Uani 1 1 d . . . H9 H 1.0487 1.1112 0.4696 0.096 Uiso 1 1 calc R . . C10 C 1.1208(4) 0.9955(4) 0.43998(13) 0.0705(16) Uani 1 1 d . . . H10 H 1.0665 1.0046 0.4211 0.085 Uiso 1 1 calc R . . C11 C 1.2608(5) 1.1010(4) 0.55836(13) 0.0757(17) Uani 1 1 d . . . H11A H 1.2789 1.0242 0.5622 0.091 Uiso 1 1 calc R . . H11B H 1.2249 1.1284 0.5794 0.091 Uiso 1 1 calc R . . C12 C 1.3751(4) 1.1619(4) 0.55334(12) 0.0622(14) Uani 1 1 d . . . H12A H 1.4143 1.1320 0.5335 0.093 Uiso 1 1 calc R . . H12B H 1.4257 1.1547 0.5741 0.093 Uiso 1 1 calc R . . H12C H 1.3581 1.2379 0.5492 0.093 Uiso 1 1 calc R . . C13 C 1.0805(5) 1.1960(6) 0.53051(16) 0.096(2) Uani 1 1 d . . . H13A H 1.0657 1.2109 0.5550 0.115 Uiso 1 1 calc R . . H13B H 1.0077 1.1673 0.5196 0.115 Uiso 1 1 calc R . . C14 C 1.1106(6) 1.3021(6) 0.51266(19) 0.112(2) Uani 1 1 d . . . H14A H 1.1827 1.3313 0.5232 0.169 Uiso 1 1 calc R . . H14B H 1.0472 1.3536 0.5154 0.169 Uiso 1 1 calc R . . H14C H 1.1211 1.2891 0.4881 0.169 Uiso 1 1 calc R . . C15 C 1.0410(3) 0.7702(3) 0.32577(10) 0.0338(10) Uani 1 1 d . . . H15 H 0.9731 0.8093 0.3311 0.041 Uiso 1 1 calc R . . C16 C 1.0414(3) 0.7050(3) 0.29635(10) 0.0303(9) Uani 1 1 d . . . C17 C 0.9369(3) 0.6930(3) 0.27392(10) 0.0343(10) Uani 1 1 d . . . H17 H 0.8729 0.7373 0.2793 0.041 Uiso 1 1 calc R . . C18 C 0.9195(3) 0.6259(3) 0.24622(10) 0.0324(10) Uani 1 1 d . . . H18 H 0.9823 0.5811 0.2403 0.039 Uiso 1 1 calc R . . C19 C 0.8105(3) 0.6179(3) 0.22481(10) 0.0321(10) Uani 1 1 d . . . C20 C 0.7972(3) 0.5394(3) 0.19823(10) 0.0326(10) Uani 1 1 d . . . H20 H 0.8597 0.4919 0.1942 0.039 Uiso 1 1 calc R . . C21 C 0.6941(3) 0.5306(3) 0.17782(10) 0.0354(10) Uani 1 1 d . . . H21 H 0.6891 0.4778 0.1602 0.043 Uiso 1 1 calc R . . C22 C 0.5969(3) 0.5983(3) 0.18283(10) 0.0302(9) Uani 1 1 d . . . C23 C 0.6094(3) 0.6767(3) 0.20990(10) 0.0372(10) Uani 1 1 d . . . H23 H 0.5464 0.7233 0.2143 0.045 Uiso 1 1 calc R . . C24 C 0.7131(3) 0.6855(3) 0.22993(11) 0.0383(10) Uani 1 1 d . . . H24 H 0.7185 0.7385 0.2475 0.046 Uiso 1 1 calc R . . C25 C 0.4855(4) 0.5163(3) 0.13261(10) 0.0403(11) Uani 1 1 d . . . H25A H 0.4027 0.4988 0.1275 0.048 Uiso 1 1 calc R . . H25B H 0.5263 0.4486 0.1387 0.048 Uiso 1 1 calc R . . C26 C 0.5378(4) 0.5629(4) 0.09990(11) 0.0568(13) Uani 1 1 d . . . H26A H 0.4932 0.6262 0.0923 0.085 Uiso 1 1 calc R . . H26B H 0.5347 0.5088 0.0816 0.085 Uiso 1 1 calc R . . H26C H 0.6190 0.5834 0.1050 0.085 Uiso 1 1 calc R . . C27 C 0.3983(3) 0.6695(3) 0.16584(11) 0.0444(11) Uani 1 1 d . . . H27A H 0.3863 0.6831 0.1906 0.053 Uiso 1 1 calc R . . H27B H 0.3255 0.6381 0.1558 0.053 Uiso 1 1 calc R . . C28 C 0.4203(4) 0.7777(4) 0.14791(12) 0.0612(14) Uani 1 1 d . . . H28A H 0.4891 0.8121 0.1588 0.092 Uiso 1 1 calc R . . H28B H 0.3525 0.8243 0.1502 0.092 Uiso 1 1 calc R . . H28C H 0.4334 0.7653 0.1234 0.092 Uiso 1 1 calc R . . C29 C 0.7305(4) 0.9750(3) 0.27763(10) 0.0341(10) Uani 1 1 d . . . C30 C 0.6358(3) 0.8421(3) 0.31004(9) 0.0282(9) Uani 1 1 d . . . C31 C 0.6470(4) 0.7669(3) 0.33956(10) 0.0355(10) Uani 1 1 d . . . H31 H 0.7221 0.7594 0.3503 0.043 Uiso 1 1 calc R . . C32 C 0.5610(4) 0.7083(3) 0.35249(10) 0.0367(10) Uani 1 1 d . . . H32 H 0.4864 0.7173 0.3415 0.044 Uiso 1 1 calc R . . C33 C 0.5674(4) 0.6305(3) 0.38209(10) 0.0329(10) Uani 1 1 d . . . C34 C 0.6739(4) 0.5982(3) 0.39879(11) 0.0450(11) Uani 1 1 d . . . H34 H 0.7446 0.6291 0.3917 0.054 Uiso 1 1 calc R . . C35 C 0.6777(4) 0.5214(4) 0.42561(11) 0.0485(12) Uani 1 1 d . . . H35 H 0.7506 0.5006 0.4358 0.058 Uiso 1 1 calc R . . C36 C 0.5743(4) 0.4750(3) 0.43746(11) 0.0432(11) Uani 1 1 d . . . C37 C 0.4671(4) 0.5099(3) 0.42139(11) 0.0459(11) Uani 1 1 d . . . H37 H 0.3960 0.4819 0.4292 0.055 Uiso 1 1 calc R . . C38 C 0.4642(4) 0.5849(3) 0.39419(11) 0.0408(11) Uani 1 1 d . . . H38 H 0.3915 0.6052 0.3838 0.049 Uiso 1 1 calc R . . C39 C 0.6896(7) 0.3305(6) 0.47072(18) 0.117(3) Uani 1 1 d . . . H39A H 0.6695 0.2545 0.4748 0.140 Uiso 1 1 calc R . . H39B H 0.7398 0.3346 0.4506 0.140 Uiso 1 1 calc R . . C40 C 0.7477(7) 0.3760(5) 0.5009(2) 0.129(3) Uani 1 1 d . . . H40A H 0.7658 0.4515 0.4965 0.193 Uiso 1 1 calc R . . H40B H 0.8200 0.3366 0.5061 0.193 Uiso 1 1 calc R . . H40C H 0.6970 0.3709 0.5205 0.193 Uiso 1 1 calc R . . C41 C 0.4695(4) 0.3626(4) 0.48085(12) 0.0544(13) Uani 1 1 d . . . H41A H 0.4136 0.4230 0.4811 0.065 Uiso 1 1 calc R . . H41B H 0.4892 0.3431 0.5051 0.065 Uiso 1 1 calc R . . C42 C 0.4106(5) 0.2669(4) 0.46293(13) 0.0790(17) Uani 1 1 d . . . H42A H 0.3908 0.2853 0.4388 0.118 Uiso 1 1 calc R . . H42B H 0.3396 0.2485 0.4747 0.118 Uiso 1 1 calc R . . H42C H 0.4637 0.2054 0.4637 0.118 Uiso 1 1 calc R . . C43 C 0.5334(3) 0.8490(3) 0.28783(10) 0.0305(9) Uani 1 1 d . . . H43 H 0.4680 0.8050 0.2919 0.037 Uiso 1 1 calc R . . C44 C 0.5307(3) 0.9213(3) 0.25999(10) 0.0294(9) Uani 1 1 d . . . C45 C 0.4334(3) 0.9409(3) 0.23446(10) 0.0319(9) Uani 1 1 d . . . H45 H 0.4457 0.9911 0.2166 0.038 Uiso 1 1 calc R . . C46 C 0.3274(3) 0.8916(3) 0.23496(10) 0.0344(10) Uani 1 1 d . . . H46 H 0.3182 0.8398 0.2526 0.041 Uiso 1 1 calc R . . C47 C 0.2251(3) 0.9094(3) 0.21126(10) 0.0333(10) Uani 1 1 d . . . C48 C 0.2205(4) 0.9843(3) 0.18381(10) 0.0361(10) Uani 1 1 d . . . H48 H 0.2873 1.0267 0.1799 0.043 Uiso 1 1 calc R . . C49 C 0.1220(4) 0.9983(3) 0.16230(11) 0.0404(11) Uani 1 1 d . . . H49 H 0.1250 1.0475 0.1437 0.048 Uiso 1 1 calc R . . C50 C 0.0158(4) 0.9405(3) 0.16739(10) 0.0366(10) Uani 1 1 d . . . C51 C 0.0198(4) 0.8656(4) 0.19526(11) 0.0482(12) Uani 1 1 d . . . H51 H -0.0476 0.8249 0.1999 0.058 Uiso 1 1 calc R . . C52 C 0.1207(4) 0.8510(3) 0.21587(11) 0.0461(12) Uani 1 1 d . . . H52 H 0.1196 0.7994 0.2339 0.055 Uiso 1 1 calc R . . C53 C -0.0829(4) 1.0249(3) 0.11485(11) 0.0459(11) Uani 1 1 d . . . H53A H -0.0370 1.0905 0.1200 0.055 Uiso 1 1 calc R . . H53B H -0.1634 1.0474 0.1084 0.055 Uiso 1 1 calc R . . C54 C -0.0310(5) 0.9677(4) 0.08379(12) 0.0651(14) Uani 1 1 d . . . H54A H 0.0474 0.9421 0.0902 0.098 Uiso 1 1 calc R . . H54B H -0.0270 1.0180 0.0645 0.098 Uiso 1 1 calc R . . H54C H -0.0803 0.9067 0.0769 0.098 Uiso 1 1 calc R . . C55 C -0.1978(4) 0.9026(4) 0.15391(12) 0.0541(13) Uani 1 1 d . . . H55A H -0.2635 0.9486 0.1458 0.065 Uiso 1 1 calc R . . H55B H -0.2033 0.8936 0.1792 0.065 Uiso 1 1 calc R . . C56 C -0.2100(4) 0.7925(4) 0.13658(14) 0.0712(15) Uani 1 1 d . . . H56A H -0.2031 0.8004 0.1116 0.107 Uiso 1 1 calc R . . H56B H -0.2862 0.7619 0.1413 0.107 Uiso 1 1 calc R . . H56C H -0.1486 0.7447 0.1457 0.107 Uiso 1 1 calc R . . C57 C 0.9185(4) 0.0911(4) 0.35923(13) 0.0567(13) Uani 1 1 d . . . H57A H 0.8884 0.1208 0.3369 0.068 Uiso 1 1 calc R . . H57B H 1.0037 0.0819 0.3579 0.068 Uiso 1 1 calc R . . C58 C 0.8920(5) 0.1698(4) 0.38881(14) 0.0782(17) Uani 1 1 d . . . H58A H 0.8076 0.1780 0.3903 0.117 Uiso 1 1 calc R . . H58B H 0.9270 0.2397 0.3842 0.117 Uiso 1 1 calc R . . H58C H 0.9245 0.1415 0.4107 0.117 Uiso 1 1 calc R . . O3 O 0.8648(3) -0.0113(3) 0.36536(8) 0.0556(9) Uani 1 1 d . . . H3A H 0.8792 -0.0534 0.3493 0.083 Uiso 1 1 calc R . . N1 N 1.2447(3) 0.7268(3) 0.34075(8) 0.0329(8) Uani 1 1 d . . . N2 N 1.1454(3) 0.6526(2) 0.28917(8) 0.0298(8) Uani 1 1 d . . . N3 N 1.1748(4) 1.1104(3) 0.52890(11) 0.0673(12) Uani 1 1 d . . . N4 N 0.4932(3) 0.5896(3) 0.16300(8) 0.0348(8) Uani 1 1 d . . . N5 N 0.7315(3) 0.9050(2) 0.30532(8) 0.0315(8) Uani 1 1 d . . . N6 N 0.6310(3) 0.9830(2) 0.25517(8) 0.0314(8) Uani 1 1 d . . . N7 N 0.5771(4) 0.3992(3) 0.46436(10) 0.0598(11) Uani 1 1 d . . . N8 N -0.0855(3) 0.9583(3) 0.14672(9) 0.0426(9) Uani 1 1 d . . . O1 O 1.3410(2) 0.6219(2) 0.30158(8) 0.0435(8) Uani 1 1 d . . . H1 H 1.3246 0.5685 0.2892 0.065 Uiso 1 1 calc R . . O2 O 0.8177(2) 1.0348(2) 0.27242(7) 0.0452(8) Uani 1 1 d . . . H2 H 0.8184 1.0509 0.2515 0.068 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 C1 0.027(2) 0.033(2) 0.035(2) 0.0007(19) 0.0010(19) -0.0003(19) C2 0.028(2) 0.030(2) 0.034(2) -0.0037(18) 0.0028(19) -0.0055(18) C3 0.034(2) 0.036(2) 0.038(3) -0.0030(19) 0.002(2) 0.0028(19) C4 0.036(2) 0.036(2) 0.038(3) -0.005(2) 0.003(2) 0.0000(19) C5 0.038(3) 0.040(2) 0.036(3) -0.008(2) -0.001(2) 0.003(2) C6 0.048(3) 0.037(2) 0.039(3) 0.001(2) -0.010(2) 0.000(2) C7 0.066(3) 0.043(3) 0.035(3) 0.001(2) -0.008(2) -0.007(2) C8 0.053(3) 0.065(3) 0.040(3) -0.013(2) 0.010(2) -0.015(3) C9 0.061(4) 0.103(4) 0.075(4) -0.047(4) -0.019(3) 0.030(3) C10 0.068(4) 0.087(4) 0.055(3) -0.037(3) -0.024(3) 0.029(3) C11 0.119(5) 0.080(4) 0.029(3) -0.011(3) 0.007(3) -0.029(4) C12 0.080(4) 0.052(3) 0.053(3) -0.006(2) -0.018(3) 0.005(3) C13 0.060(4) 0.145(6) 0.084(5) -0.058(5) 0.008(3) -0.003(4) C14 0.106(6) 0.108(6) 0.121(6) -0.040(5) -0.024(5) 0.031(5) C15 0.027(2) 0.036(2) 0.038(3) -0.006(2) 0.0038(19) 0.0007(18) C16 0.028(2) 0.034(2) 0.030(2) 0.0041(18) 0.0011(18) 0.0021(17) C17 0.026(2) 0.038(2) 0.038(3) -0.004(2) -0.0024(19) 0.0036(18) C18 0.022(2) 0.033(2) 0.042(3) 0.0020(19) 0.0033(19) 0.0008(17) C19 0.031(2) 0.032(2) 0.033(2) -0.0016(18) 0.0003(19) 0.0007(18) C20 0.030(2) 0.032(2) 0.036(2) -0.0036(19) 0.0048(19) 0.0002(17) C21 0.035(2) 0.035(2) 0.036(3) -0.0079(19) 0.001(2) -0.0031(19) C22 0.029(2) 0.033(2) 0.028(2) 0.0002(18) -0.0016(18) -0.0013(18) C23 0.030(2) 0.042(2) 0.039(3) -0.009(2) -0.001(2) 0.0074(19) C24 0.028(2) 0.045(2) 0.042(3) -0.012(2) -0.001(2) 0.0031(19) C25 0.042(3) 0.044(2) 0.035(3) -0.008(2) -0.006(2) -0.001(2) C26 0.077(4) 0.057(3) 0.038(3) -0.004(2) 0.010(3) -0.005(3) C27 0.028(2) 0.060(3) 0.045(3) -0.001(2) -0.007(2) 0.003(2) C28 0.066(4) 0.059(3) 0.058(3) 0.000(3) 0.001(3) 0.022(3) C29 0.031(2) 0.038(2) 0.034(3) 0.001(2) 0.001(2) -0.0043(19) C30 0.029(2) 0.030(2) 0.025(2) -0.0031(17) 0.0023(18) 0.0023(18) C31 0.032(2) 0.037(2) 0.038(3) -0.002(2) 0.0045(19) -0.0009(19) C32 0.035(2) 0.035(2) 0.039(3) -0.008(2) -0.005(2) 0.0039(19) C33 0.035(2) 0.034(2) 0.029(2) -0.0030(18) -0.0036(19) 0.0031(19) C34 0.046(3) 0.048(3) 0.041(3) 0.000(2) 0.009(2) -0.002(2) C35 0.049(3) 0.058(3) 0.039(3) 0.013(2) 0.006(2) 0.015(2) C36 0.054(3) 0.042(2) 0.034(3) 0.007(2) 0.004(2) 0.007(2) C37 0.047(3) 0.047(3) 0.044(3) 0.009(2) 0.002(2) -0.002(2) C38 0.042(3) 0.039(2) 0.041(3) 0.002(2) -0.006(2) -0.004(2) C39 0.151(7) 0.106(5) 0.089(5) 0.058(4) -0.050(5) -0.041(5) C40 0.124(7) 0.083(5) 0.183(9) 0.032(5) 0.064(6) 0.026(4) C41 0.072(4) 0.051(3) 0.041(3) 0.010(2) 0.016(3) -0.001(3) C42 0.116(5) 0.061(3) 0.060(4) 0.002(3) 0.014(3) -0.018(3) C43 0.031(2) 0.029(2) 0.031(2) -0.0024(18) 0.0035(18) -0.0016(17) C44 0.029(2) 0.032(2) 0.026(2) -0.0037(18) 0.0006(18) 0.0012(18) C45 0.033(2) 0.035(2) 0.027(2) 0.0001(18) 0.0009(18) 0.0015(18) C46 0.037(3) 0.034(2) 0.033(2) 0.0011(18) 0.0031(19) -0.0036(19) C47 0.027(2) 0.039(2) 0.034(2) 0.0004(19) -0.0015(19) -0.0014(19) C48 0.032(2) 0.036(2) 0.040(3) 0.005(2) -0.001(2) -0.0028(18) C49 0.040(3) 0.041(2) 0.041(3) 0.008(2) 0.002(2) -0.002(2) C50 0.033(2) 0.045(2) 0.032(2) -0.001(2) -0.0010(19) 0.003(2) C51 0.036(3) 0.066(3) 0.042(3) 0.019(2) -0.005(2) -0.019(2) C52 0.042(3) 0.056(3) 0.040(3) 0.018(2) -0.010(2) -0.016(2) C53 0.038(3) 0.051(3) 0.048(3) 0.006(2) -0.011(2) 0.005(2) C54 0.085(4) 0.067(3) 0.044(3) 0.005(3) 0.011(3) -0.003(3) C55 0.039(3) 0.066(3) 0.056(3) 0.004(3) -0.010(2) 0.002(2) C56 0.065(4) 0.067(3) 0.082(4) 0.003(3) 0.002(3) -0.016(3) C57 0.044(3) 0.066(3) 0.060(3) -0.005(3) -0.004(2) -0.005(2) C58 0.067(4) 0.085(4) 0.081(4) -0.026(3) -0.018(3) 0.017(3) O3 0.055(2) 0.064(2) 0.048(2) -0.0062(16) -0.0014(16) -0.0047(16) N1 0.0291(19) 0.0394(19) 0.030(2) -0.0051(16) -0.0013(15) -0.0037(15) N2 0.0249(18) 0.0344(18) 0.0299(19) 0.0015(15) -0.0029(15) -0.0007(14) N3 0.074(3) 0.078(3) 0.051(3) -0.033(2) 0.007(2) -0.009(2) N4 0.0283(19) 0.043(2) 0.033(2) -0.0034(16) -0.0027(16) -0.0052(16) N5 0.032(2) 0.0334(18) 0.029(2) 0.0036(15) 0.0024(15) -0.0014(15) N6 0.0201(18) 0.0391(19) 0.035(2) -0.0017(15) -0.0002(15) -0.0025(14) N7 0.067(3) 0.059(3) 0.053(3) 0.027(2) 0.008(2) 0.018(2) N8 0.031(2) 0.055(2) 0.041(2) 0.0084(18) -0.0072(17) -0.0072(17) O1 0.0311(17) 0.0552(19) 0.0437(19) -0.0206(15) -0.0060(14) -0.0005(14) O2 0.0369(18) 0.065(2) 0.0336(18) 0.0153(15) -0.0034(14) -0.0133(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.250(4) . ? C1 N1 1.357(5) . ? C1 N2 1.396(4) . ? C2 N1 1.339(5) . ? C2 C15 1.394(5) . ? C2 C3 1.454(5) . ? C3 C4 1.340(5) . ? C3 H3 0.9300 . ? C4 C5 1.459(5) . ? C4 H4 0.9300 . ? C5 C10 1.374(6) . ? C5 C6 1.381(5) . ? C6 C7 1.378(6) . ? C6 H6 0.9300 . ? C7 C8 1.396(6) . ? C7 H7 0.9300 . ? C8 N3 1.376(5) . ? C8 C9 1.408(6) . ? C9 C10 1.371(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 N3 1.456(6) . ? C11 C12 1.506(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N3 1.493(7) . ? C13 C14 1.508(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.372(5) . ? C15 H15 0.9300 . ? C16 N2 1.372(4) . ? C16 C17 1.434(5) . ? C17 C18 1.342(5) . ? C17 H17 0.9300 . ? C18 C19 1.449(5) . ? C18 H18 0.9300 . ? C19 C24 1.394(5) . ? C19 C20 1.396(5) . ? C20 C21 1.376(5) . ? C20 H20 0.9300 . ? C21 C22 1.391(5) . ? C21 H21 0.9300 . ? C22 N4 1.370(4) . ? C22 C23 1.408(5) . ? C23 C24 1.373(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 N4 1.460(5) . ? C25 C26 1.508(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 N4 1.455(5) . ? C27 C28 1.512(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O2 1.246(4) . ? C29 N5 1.355(5) . ? C29 N6 1.386(5) . ? C30 N5 1.342(4) . ? C30 C43 1.404(5) . ? C30 C31 1.451(5) . ? C31 C32 1.316(5) . ? C31 H31 0.9300 . ? C32 C33 1.472(5) . ? C32 H32 0.9300 . ? C33 C38 1.384(5) . ? C33 C34 1.392(5) . ? C34 C35 1.384(6) . ? C34 H34 0.9300 . ? C35 C36 1.386(6) . ? C35 H35 0.9300 . ? C36 N7 1.378(5) . ? C36 C37 1.399(5) . ? C37 C38 1.380(5) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.410(9) . ? C39 N7 1.532(8) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 N7 1.456(5) . ? C41 C42 1.495(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.377(5) . ? C43 H43 0.9300 . ? C44 N6 1.377(4) . ? C44 C45 1.454(5) . ? C45 C46 1.339(5) . ? C45 H45 0.9300 . ? C46 C47 1.450(5) . ? C46 H46 0.9300 . ? C47 C48 1.387(5) . ? C47 C52 1.393(5) . ? C48 C49 1.362(5) . ? C48 H48 0.9300 . ? C49 C50 1.410(5) . ? C49 H49 0.9300 . ? C50 N8 1.376(5) . ? C50 C51 1.398(5) . ? C51 C52 1.366(5) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 N8 1.459(5) . ? C53 C54 1.509(6) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 N8 1.472(5) . ? C55 C56 1.502(6) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 O3 1.414(5) . ? C57 C58 1.517(6) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? O3 H3A 0.8200 . ? O1 H1 0.8200 . ? O2 H2 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 N1 121.2(3) . . ? O1 C1 N2 117.9(3) . . ? N1 C1 N2 120.9(3) . . ? N1 C2 C15 123.0(4) . . ? N1 C2 C3 119.7(3) . . ? C15 C2 C3 117.2(4) . . ? C4 C3 C2 126.6(4) . . ? C4 C3 H3 116.7 . . ? C2 C3 H3 116.7 . . ? C3 C4 C5 125.5(4) . . ? C3 C4 H4 117.3 . . ? C5 C4 H4 117.3 . . ? C10 C5 C6 116.2(4) . . ? C10 C5 C4 121.7(4) . . ? C6 C5 C4 122.1(4) . . ? C7 C6 C5 122.1(4) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C6 C7 C8 122.1(4) . . ? C6 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? N3 C8 C7 122.8(5) . . ? N3 C8 C9 121.9(5) . . ? C7 C8 C9 115.3(4) . . ? C10 C9 C8 121.4(5) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C5 123.0(5) . . ? C9 C10 H10 118.5 . . ? C5 C10 H10 118.5 . . ? N3 C11 C12 114.3(4) . . ? N3 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? N3 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 114.2(5) . . ? N3 C13 H13A 108.7 . . ? C14 C13 H13A 108.7 . . ? N3 C13 H13B 108.7 . . ? C14 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C2 119.6(4) . . ? C16 C15 H15 120.2 . . ? C2 C15 H15 120.2 . . ? C15 C16 N2 117.6(3) . . ? C15 C16 C17 121.0(4) . . ? N2 C16 C17 121.5(3) . . ? C18 C17 C16 128.3(4) . . ? C18 C17 H17 115.9 . . ? C16 C17 H17 115.9 . . ? C17 C18 C19 125.1(4) . . ? C17 C18 H18 117.4 . . ? C19 C18 H18 117.4 . . ? C24 C19 C20 116.4(4) . . ? C24 C19 C18 122.5(4) . . ? C20 C19 C18 121.1(3) . . ? C21 C20 C19 121.7(4) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C22 121.9(4) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? N4 C22 C21 122.5(3) . . ? N4 C22 C23 120.9(3) . . ? C21 C22 C23 116.6(4) . . ? C24 C23 C22 121.1(4) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C19 122.3(4) . . ? C23 C24 H24 118.9 . . ? C19 C24 H24 118.9 . . ? N4 C25 C26 114.0(3) . . ? N4 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? N4 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N4 C27 C28 114.8(3) . . ? N4 C27 H27A 108.6 . . ? C28 C27 H27A 108.6 . . ? N4 C27 H27B 108.6 . . ? C28 C27 H27B 108.6 . . ? H27A C27 H27B 107.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O2 C29 N5 120.7(4) . . ? O2 C29 N6 119.0(4) . . ? N5 C29 N6 120.3(3) . . ? N5 C30 C43 122.1(3) . . ? N5 C30 C31 114.8(3) . . ? C43 C30 C31 123.1(3) . . ? C32 C31 C30 126.1(4) . . ? C32 C31 H31 116.9 . . ? C30 C31 H31 116.9 . . ? C31 C32 C33 128.4(4) . . ? C31 C32 H32 115.8 . . ? C33 C32 H32 115.8 . . ? C38 C33 C34 117.1(4) . . ? C38 C33 C32 119.7(4) . . ? C34 C33 C32 123.2(4) . . ? C35 C34 C33 121.9(4) . . ? C35 C34 H34 119.1 . . ? C33 C34 H34 119.1 . . ? C34 C35 C36 120.9(4) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? N7 C36 C35 121.4(4) . . ? N7 C36 C37 121.5(4) . . ? C35 C36 C37 117.2(4) . . ? C38 C37 C36 121.5(4) . . ? C38 C37 H37 119.2 . . ? C36 C37 H37 119.2 . . ? C37 C38 C33 121.3(4) . . ? C37 C38 H38 119.3 . . ? C33 C38 H38 119.3 . . ? C40 C39 N7 105.5(7) . . ? C40 C39 H39A 110.6 . . ? N7 C39 H39A 110.6 . . ? C40 C39 H39B 110.6 . . ? N7 C39 H39B 110.6 . . ? H39A C39 H39B 108.8 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N7 C41 C42 114.0(4) . . ? N7 C41 H41A 108.8 . . ? C42 C41 H41A 108.8 . . ? N7 C41 H41B 108.8 . . ? C42 C41 H41B 108.8 . . ? H41A C41 H41B 107.6 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C30 119.5(4) . . ? C44 C43 H43 120.3 . . ? C30 C43 H43 120.3 . . ? N6 C44 C43 117.3(3) . . ? N6 C44 C45 115.0(3) . . ? C43 C44 C45 127.7(4) . . ? C46 C45 C44 124.5(4) . . ? C46 C45 H45 117.8 . . ? C44 C45 H45 117.8 . . ? C45 C46 C47 127.7(4) . . ? C45 C46 H46 116.1 . . ? C47 C46 H46 116.1 . . ? C48 C47 C52 115.2(4) . . ? C48 C47 C46 124.8(4) . . ? C52 C47 C46 120.0(4) . . ? C49 C48 C47 122.6(4) . . ? C49 C48 H48 118.7 . . ? C47 C48 H48 118.7 . . ? C48 C49 C50 122.1(4) . . ? C48 C49 H49 119.0 . . ? C50 C49 H49 119.0 . . ? N8 C50 C51 122.5(4) . . ? N8 C50 C49 122.2(4) . . ? C51 C50 C49 115.4(4) . . ? C52 C51 C50 121.4(4) . . ? C52 C51 H51 119.3 . . ? C50 C51 H51 119.3 . . ? C51 C52 C47 123.3(4) . . ? C51 C52 H52 118.4 . . ? C47 C52 H52 118.4 . . ? N8 C53 C54 114.3(3) . . ? N8 C53 H53A 108.7 . . ? C54 C53 H53A 108.7 . . ? N8 C53 H53B 108.7 . . ? C54 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N8 C55 C56 113.4(4) . . ? N8 C55 H55A 108.9 . . ? C56 C55 H55A 108.9 . . ? N8 C55 H55B 108.9 . . ? C56 C55 H55B 108.9 . . ? H55A C55 H55B 107.7 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O3 C57 C58 109.9(4) . . ? O3 C57 H57A 109.7 . . ? C58 C57 H57A 109.7 . . ? O3 C57 H57B 109.7 . . ? C58 C57 H57B 109.7 . . ? H57A C57 H57B 108.2 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 O3 H3A 109.5 . . ? C2 N1 C1 117.6(3) . . ? C16 N2 C1 121.1(3) . . ? C8 N3 C11 120.3(4) . . ? C8 N3 C13 120.9(4) . . ? C11 N3 C13 118.5(4) . . ? C22 N4 C27 121.4(3) . . ? C22 N4 C25 120.4(3) . . ? C27 N4 C25 116.7(3) . . ? C30 N5 C29 118.9(3) . . ? C44 N6 C29 121.9(3) . . ? C36 N7 C41 122.0(4) . . ? C36 N7 C39 118.6(4) . . ? C41 N7 C39 117.5(4) . . ? C50 N8 C53 121.2(3) . . ? C50 N8 C55 121.4(3) . . ? C53 N8 C55 117.1(3) . . ? C1 O1 H1 109.5 . . ? C29 O2 H2 109.5 . . ? 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 C2 C3 C4 -7.6(6) . . . . ? C15 C2 C3 C4 171.8(4) . . . . ? C2 C3 C4 C5 179.1(4) . . . . ? C3 C4 C5 C10 -10.8(7) . . . . ? C3 C4 C5 C6 168.9(4) . . . . ? C10 C5 C6 C7 0.2(6) . . . . ? C4 C5 C6 C7 -179.4(4) . . . . ? C5 C6 C7 C8 0.4(7) . . . . ? C6 C7 C8 N3 177.5(4) . . . . ? C6 C7 C8 C9 -1.1(7) . . . . ? N3 C8 C9 C10 -177.4(5) . . . . ? C7 C8 C9 C10 1.2(8) . . . . ? C8 C9 C10 C5 -0.6(9) . . . . ? C6 C5 C10 C9 -0.1(8) . . . . ? C4 C5 C10 C9 179.5(5) . . . . ? N1 C2 C15 C16 2.6(6) . . . . ? C3 C2 C15 C16 -176.7(3) . . . . ? C2 C15 C16 N2 -2.3(5) . . . . ? C2 C15 C16 C17 178.0(3) . . . . ? C15 C16 C17 C18 -173.7(4) . . . . ? N2 C16 C17 C18 6.6(6) . . . . ? C16 C17 C18 C19 179.7(4) . . . . ? C17 C18 C19 C24 3.9(6) . . . . ? C17 C18 C19 C20 -174.7(4) . . . . ? C24 C19 C20 C21 1.0(6) . . . . ? C18 C19 C20 C21 179.7(4) . . . . ? C19 C20 C21 C22 -0.8(6) . . . . ? C20 C21 C22 N4 -179.2(3) . . . . ? C20 C21 C22 C23 0.0(6) . . . . ? N4 C22 C23 C24 179.8(4) . . . . ? C21 C22 C23 C24 0.5(6) . . . . ? C22 C23 C24 C19 -0.3(6) . . . . ? C20 C19 C24 C23 -0.4(6) . . . . ? C18 C19 C24 C23 -179.1(4) . . . . ? N5 C30 C31 C32 169.9(4) . . . . ? C43 C30 C31 C32 -10.4(6) . . . . ? C30 C31 C32 C33 179.5(4) . . . . ? C31 C32 C33 C38 173.3(4) . . . . ? C31 C32 C33 C34 -7.5(6) . . . . ? C38 C33 C34 C35 1.9(6) . . . . ? C32 C33 C34 C35 -177.3(4) . . . . ? C33 C34 C35 C36 -1.4(7) . . . . ? C34 C35 C36 N7 -179.4(4) . . . . ? C34 C35 C36 C37 -0.6(6) . . . . ? N7 C36 C37 C38 -179.3(4) . . . . ? C35 C36 C37 C38 1.9(6) . . . . ? C36 C37 C38 C33 -1.3(6) . . . . ? C34 C33 C38 C37 -0.6(6) . . . . ? C32 C33 C38 C37 178.6(4) . . . . ? N5 C30 C43 C44 0.8(5) . . . . ? C31 C30 C43 C44 -178.9(3) . . . . ? C30 C43 C44 N6 0.8(5) . . . . ? C30 C43 C44 C45 -179.4(3) . . . . ? N6 C44 C45 C46 -178.2(3) . . . . ? C43 C44 C45 C46 1.9(6) . . . . ? C44 C45 C46 C47 177.7(4) . . . . ? C45 C46 C47 C48 -1.2(6) . . . . ? C45 C46 C47 C52 -179.5(4) . . . . ? C52 C47 C48 C49 -1.4(6) . . . . ? C46 C47 C48 C49 -179.8(4) . . . . ? C47 C48 C49 C50 2.7(6) . . . . ? C48 C49 C50 N8 176.9(4) . . . . ? C48 C49 C50 C51 -1.9(6) . . . . ? N8 C50 C51 C52 -178.6(4) . . . . ? C49 C50 C51 C52 0.2(6) . . . . ? C50 C51 C52 C47 1.0(7) . . . . ? C48 C47 C52 C51 -0.4(6) . . . . ? C46 C47 C52 C51 178.1(4) . . . . ? C15 C2 N1 C1 0.7(5) . . . . ? C3 C2 N1 C1 -180.0(3) . . . . ? O1 C1 N1 C2 176.0(3) . . . . ? N2 C1 N1 C2 -4.1(5) . . . . ? C15 C16 N2 C1 -1.0(5) . . . . ? C17 C16 N2 C1 178.7(3) . . . . ? O1 C1 N2 C16 -175.8(3) . . . . ? N1 C1 N2 C16 4.4(5) . . . . ? C7 C8 N3 C11 4.3(7) . . . . ? C9 C8 N3 C11 -177.2(5) . . . . ? C7 C8 N3 C13 177.4(5) . . . . ? C9 C8 N3 C13 -4.1(7) . . . . ? C12 C11 N3 C8 77.8(6) . . . . ? C12 C11 N3 C13 -95.5(6) . . . . ? C14 C13 N3 C8 -78.8(6) . . . . ? C14 C13 N3 C11 94.5(6) . . . . ? C21 C22 N4 C27 -172.5(4) . . . . ? C23 C22 N4 C27 8.3(5) . . . . ? C21 C22 N4 C25 -7.4(5) . . . . ? C23 C22 N4 C25 173.4(4) . . . . ? C28 C27 N4 C22 75.8(5) . . . . ? C28 C27 N4 C25 -89.8(4) . . . . ? C26 C25 N4 C22 -80.1(4) . . . . ? C26 C25 N4 C27 85.6(4) . . . . ? C43 C30 N5 C29 -2.0(5) . . . . ? C31 C30 N5 C29 177.7(3) . . . . ? O2 C29 N5 C30 179.9(3) . . . . ? N6 C29 N5 C30 1.6(5) . . . . ? C43 C44 N6 C29 -1.2(5) . . . . ? C45 C44 N6 C29 179.0(3) . . . . ? O2 C29 N6 C44 -178.4(3) . . . . ? N5 C29 N6 C44 0.0(5) . . . . ? C35 C36 N7 C41 170.2(4) . . . . ? C37 C36 N7 C41 -8.6(7) . . . . ? C35 C36 N7 C39 -25.7(7) . . . . ? C37 C36 N7 C39 155.5(5) . . . . ? C42 C41 N7 C36 88.2(5) . . . . ? C42 C41 N7 C39 -76.1(6) . . . . ? C40 C39 N7 C36 104.1(6) . . . . ? C40 C39 N7 C41 -91.1(6) . . . . ? C51 C50 N8 C53 -171.2(4) . . . . ? C49 C50 N8 C53 10.1(6) . . . . ? C51 C50 N8 C55 2.9(6) . . . . ? C49 C50 N8 C55 -175.8(4) . . . . ? C54 C53 N8 C50 76.8(5) . . . . ? C54 C53 N8 C55 -97.5(5) . . . . ? C56 C55 N8 C50 -87.1(5) . . . . ? C56 C55 N8 C53 87.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.661 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.146