# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1815 data_TKA128 _audit_creation_date 97-01-28 _audit_creation_method CRYSTALS #========================================================================== _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 13.1768(21) _cell_angle_alpha 90 _cell_length_b 7.7443(7) _cell_angle_beta 105.38(1) _cell_length_c 21.4713(16) _cell_angle_gamma 90 _cell_volume 2112.6(4) _symmetry_cell_setting 'monoclinic ' _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,y+1/2,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0170 0.0090 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0470 0.0320 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0290 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C25 H27 N3 O ' _chemical_formula_moiety ' C25 H27 N3 O ' _chemical_compound_source ; ? ; _chemical_formula_weight 385.511 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 22 _cell_measurement_theta_max 43 _cell_measurement_temperature 293 _cell_formula_units_Z 4 _exptl_crystal_description ' cube ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.56 _exptl_crystal_density_diffrn 1.21 _exptl_crystal_density_meas ? _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.55 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '\y scan' _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time 120 _diffrn_standards_interval_count ? _diffrn_standards_number 3 _diffrn_standards_decay_% 7.53 _diffrn_ambient_temperature 293 _diffrn_reflns_number 4314 _reflns_number_total 4199 _diffrn_reflns_av_R_equivalents 0.01 _reflns_number_observed 3458 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 74.33 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 0 _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 9 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.32 _refine_diff_density_max 0.27 _refine_ls_number_reflns 3458 _refine_ls_number_parameters 525 _refine_ls_R_factor_obs 0.0651 _refine_ls_wR_factor_obs 0.0786 _refine_ls_goodness_of_fit_obs 0.8879 _refine_ls_shift/esd_max 0.028897 _refine_ls_abs_structure_details 'not determined' _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method 2\q/\w # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type N1 0.4593(3) -0.4083(6) 0.6794(2) 0.0603 1.0000 Uani C1 0.3786(3) -0.4832(7) 0.6377(2) 0.0623 1.0000 Uani C2 0.2890(3) -0.5400(7) 0.6522(2) 0.0675 1.0000 Uani C3 0.2831(3) -0.5195(8) 0.7151(2) 0.0665 1.0000 Uani C4 0.3658(3) -0.4441(7) 0.7595(2) 0.0591 1.0000 Uani C5 0.4522(3) -0.3874(6) 0.7404(2) 0.0509 1.0000 Uani N2 0.5421(2) -0.2990(5) 0.8481(1) 0.0503 1.0000 Uani C6 0.5441(3) -0.3043(6) 0.7863(2) 0.0484 1.0000 Uani C7 0.6261(3) -0.2332(6) 0.7647(2) 0.0548 1.0000 Uani C8 0.7088(3) -0.1552(7) 0.8094(2) 0.0587 1.0000 Uani C9 0.7080(3) -0.1529(6) 0.8734(2) 0.0556 1.0000 Uani C10 0.6227(3) -0.2247(6) 0.8909(2) 0.0522 1.0000 Uani N3 0.6843(2) -0.1158(5) 0.9995(1) 0.0512 1.0000 Uani C11 0.6172(3) -0.2232(6) 0.9594(2) 0.0494 1.0000 Uani C12 0.5456(3) -0.3252(7) 0.9799(2) 0.0627 1.0000 Uani C13 0.5454(3) -0.3175(6) 1.0442(2) 0.0613 1.0000 Uani C14 0.6136(3) -0.2109(7) 1.0858(2) 0.0570 1.0000 Uani C15 0.6806(3) -0.1097(6) 1.0600(2) 0.0506 1.0000 Uani O1 0.7453(2) -0.0004(5) 1.1017(1) 0.0606 1.0000 Uani C16 0.7982(3) 0.1302(7) 1.0729(2) 0.0584 1.0000 Uani C17 0.8983(5) 0.063(1) 1.0572(4) 0.1153 1.0000 Uani C18 0.9833(4) 0.187(1) 1.0955(4) 0.1065 1.0000 Uani C19 1.0035(5) 0.139(1) 1.1664(5) 0.1300 1.0000 Uani C20 0.9054(5) 0.194(1) 1.1827(2) 0.0958 1.0000 Uani C21 0.8372(3) 0.2733(6) 1.1210(2) 0.0584 1.0000 Uani C22 0.7496(5) 0.3881(9) 1.1305(4) 0.1045 1.0000 Uani C23 0.9225(4) 0.3606(8) 1.0920(2) 0.0722 1.0000 Uani C24 0.8797(6) 0.429(1) 1.0249(3) 0.1310 1.0000 Uani C25 0.9878(5) 0.502(1) 1.1322(3) 0.0961 1.0000 Uani N51 0.5624(3) 0.2210(6) 0.8218(2) 0.0604 1.0000 Uani C51 0.6459(4) 0.2941(8) 0.8620(2) 0.0714 1.0000 Uani C52 0.7304(3) 0.3557(8) 0.8425(2) 0.0681 1.0000 Uani C53 0.7301(3) 0.3399(7) 0.7788(2) 0.0668 1.0000 Uani C54 0.6450(3) 0.2631(6) 0.7365(2) 0.0560 1.0000 Uani C55 0.5621(3) 0.2057(6) 0.7597(2) 0.0498 1.0000 Uani N52 0.4653(2) 0.1175(5) 0.6530(1) 0.0489 1.0000 Uani C56 0.4689(3) 0.1218(6) 0.7159(2) 0.0486 1.0000 Uani C57 0.3892(3) 0.0477(6) 0.7401(2) 0.0549 1.0000 Uani C58 0.3051(3) -0.0271(7) 0.6974(2) 0.0596 1.0000 Uani C59 0.3003(3) -0.0321(6) 0.6324(2) 0.0552 1.0000 Uani C60 0.3815(3) 0.0443(6) 0.6119(2) 0.0473 1.0000 Uani N53 0.3074(2) -0.0586(5) 0.5029(1) 0.0506 1.0000 Uani C61 0.3788(3) 0.0459(6) 0.5418(2) 0.0487 1.0000 Uani C62 0.4462(3) 0.1519(6) 0.5191(2) 0.0534 1.0000 Uani C63 0.4397(3) 0.1481(7) 0.4533(2) 0.0610 1.0000 Uani C64 0.3689(3) 0.0412(6) 0.4133(2) 0.0548 1.0000 Uani C65 0.3037(3) -0.0567(6) 0.4403(2) 0.0511 1.0000 Uani O51 0.2325(2) -0.1606(4) 0.3995(1) 0.0599 1.0000 Uani C66 0.1745(3) -0.2832(6) 0.4285(2) 0.0545 1.0000 Uani C67 0.2434(3) -0.4300(7) 0.4626(2) 0.0653 1.0000 Uani C68 0.1872(4) -0.5914(7) 0.4272(2) 0.0689 1.0000 Uani C69 0.2079(4) -0.5951(9) 0.3611(3) 0.0852 1.0000 Uani C70 0.1401(4) -0.4449(8) 0.3258(2) 0.0689 1.0000 Uani C71 0.0879(3) -0.3706(6) 0.3757(2) 0.0558 1.0000 Uani C72 -0.0057(4) -0.256(1) 0.3470(3) 0.0933 1.0000 Uani C73 0.0701(3) -0.5353(7) 0.4123(2) 0.0604 1.0000 Uani C74 0.0299(4) -0.5028(9) 0.4718(2) 0.0850 1.0000 Uani C75 -0.0051(4) -0.669(1) 0.3712(3) 0.0901 1.0000 Uani H11 0.3833 -0.4986 0.5942 0.0601 1.0000 Uiso H21 0.2326 -0.5919 0.6199 0.0644 1.0000 Uiso H31 0.2219 -0.5575 0.7275 0.0662 1.0000 Uiso H41 0.3635 -0.4309 0.8036 0.0588 1.0000 Uiso H71 0.6251 -0.2382 0.7198 0.0560 1.0000 Uiso H81 0.7657 -0.1036 0.7959 0.0594 1.0000 Uiso H91 0.7654 -0.1025 0.9055 0.0558 1.0000 Uiso H121 0.4975 -0.3992 0.9503 0.0620 1.0000 Uiso H131 0.4970 -0.3874 1.0596 0.0628 1.0000 Uiso H141 0.6155 -0.2055 1.1308 0.0576 1.0000 Uiso H161 0.7448 0.1643 1.0350 0.0573 1.0000 Uiso H171 0.9131 -0.0541 1.0717 0.1208 1.0000 Uiso H172 0.8924 0.0691 1.0118 0.1208 1.0000 Uiso H181 1.0462 0.1871 1.0809 0.0986 1.0000 Uiso H191 1.0636 0.2001 1.1922 0.1094 1.0000 Uiso H192 1.0144 0.0173 1.1724 0.1094 1.0000 Uiso H201 0.9210 0.2784 1.2169 0.0869 1.0000 Uiso H202 0.8708 0.0970 1.1956 0.0869 1.0000 Uiso H221 0.7787 0.4765 1.1614 0.1069 1.0000 Uiso H222 0.7005 0.3202 1.1460 0.1069 1.0000 Uiso H223 0.7141 0.4406 1.0901 0.1069 1.0000 Uiso H241 0.8378 0.3410 0.9984 0.1205 1.0000 Uiso H242 0.8369 0.5283 1.0259 0.1205 1.0000 Uiso H243 0.9369 0.4599 1.0073 0.1205 1.0000 Uiso H251 1.0162 0.4611 1.1756 0.0945 1.0000 Uiso H252 0.9444 0.6010 1.1326 0.0945 1.0000 Uiso H253 1.0444 0.5326 1.1140 0.0945 1.0000 Uiso H511 0.6471 0.3044 0.9067 0.0674 1.0000 Uiso H521 0.7887 0.4089 0.8729 0.0654 1.0000 Uiso H531 0.7882 0.3816 0.7640 0.0667 1.0000 Uiso H541 0.6430 0.2496 0.6918 0.0562 1.0000 Uiso H571 0.3940 0.0498 0.7855 0.0552 1.0000 Uiso H581 0.2493 -0.0763 0.7126 0.0608 1.0000 Uiso H591 0.2423 -0.0869 0.6022 0.0546 1.0000 Uiso H621 0.4958 0.2257 0.5479 0.0540 1.0000 Uiso H631 0.4848 0.2204 0.4360 0.0629 1.0000 Uiso H641 0.3645 0.0344 0.3680 0.0558 1.0000 Uiso H661 0.1494 -0.2136 0.4583 0.0540 1.0000 Uiso H671 0.2458 -0.4329 0.5077 0.0613 1.0000 Uiso H672 0.3136 -0.4203 0.4579 0.0613 1.0000 Uiso H681 0.2074 -0.6979 0.4500 0.0668 1.0000 Uiso H691 0.2810 -0.5763 0.3641 0.0863 1.0000 Uiso H692 0.1860 -0.7029 0.3397 0.0863 1.0000 Uiso H701 0.1832 -0.3594 0.3128 0.0673 1.0000 Uiso H702 0.0881 -0.4859 0.2885 0.0673 1.0000 Uiso H721 -0.0563 -0.3194 0.3145 0.0866 1.0000 Uiso H722 -0.0373 -0.2206 0.3803 0.0866 1.0000 Uiso H723 0.0170 -0.1566 0.3278 0.0866 1.0000 Uiso H741 0.0743 -0.4197 0.4992 0.0886 1.0000 Uiso H742 0.0309 -0.6090 0.4950 0.0886 1.0000 Uiso H743 -0.0408 -0.4593 0.4584 0.0886 1.0000 Uiso H751 0.0168 -0.6942 0.3330 0.0885 1.0000 Uiso H752 -0.0036 -0.7729 0.3958 0.0885 1.0000 Uiso H753 -0.0753 -0.6233 0.3593 0.0885 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.055(2) 0.079(3) 0.046(2) -0.001(2) 0.013(1) 0.007(2) C1 0.062(2) 0.076(3) 0.046(2) -0.002(2) 0.009(2) 0.006(2) C2 0.060(2) 0.080(3) 0.056(2) -0.007(2) 0.003(2) -0.005(2) C3 0.056(2) 0.075(3) 0.069(3) -0.003(3) 0.017(2) -0.010(2) C4 0.058(2) 0.068(3) 0.052(2) -0.003(2) 0.015(2) -0.004(2) C5 0.051(2) 0.053(2) 0.047(2) 0.002(2) 0.010(2) 0.002(2) N2 0.047(1) 0.058(2) 0.047(2) -0.004(2) 0.012(1) -0.004(2) C6 0.044(2) 0.051(2) 0.050(2) -0.005(2) 0.013(1) 0.003(2) C7 0.055(2) 0.058(2) 0.055(2) -0.003(2) 0.021(2) -0.003(2) C8 0.049(2) 0.065(3) 0.066(2) -0.003(2) 0.022(2) -0.003(2) C9 0.051(2) 0.061(3) 0.056(2) -0.007(2) 0.016(2) -0.004(2) C10 0.047(2) 0.055(2) 0.055(2) -0.006(2) 0.015(2) -0.004(2) N3 0.046(1) 0.060(2) 0.048(2) -0.005(2) 0.012(1) -0.007(2) C11 0.046(2) 0.051(2) 0.051(2) 0.001(2) 0.013(1) 0.004(2) C12 0.059(2) 0.071(3) 0.057(2) -0.005(2) 0.013(2) -0.011(2) C13 0.063(2) 0.060(3) 0.065(2) 0.001(2) 0.025(2) -0.010(2) C14 0.059(2) 0.063(3) 0.052(2) 0.002(2) 0.019(2) -0.004(2) C15 0.045(2) 0.056(2) 0.048(2) -0.002(2) 0.009(1) 0.006(2) O1 0.062(1) 0.070(2) 0.050(1) -0.009(1) 0.016(1) -0.012(2) C16 0.051(2) 0.083(3) 0.044(2) -0.014(2) 0.018(2) -0.014(2) C17 0.090(4) 0.119(5) 0.165(6) -0.069(5) 0.083(4) -0.029(4) C18 0.050(2) 0.122(5) 0.156(6) -0.050(5) 0.042(3) -0.022(3) C19 0.064(3) 0.116(6) 0.177(8) 0.027(6) -0.027(4) -0.018(4) C20 0.099(4) 0.115(5) 0.058(3) -0.000(3) -0.007(2) -0.039(4) C21 0.060(2) 0.069(3) 0.049(2) -0.009(2) 0.019(2) -0.008(2) C22 0.102(4) 0.081(4) 0.147(5) -0.034(4) 0.063(4) -0.009(4) C23 0.069(3) 0.093(4) 0.057(2) -0.018(3) 0.021(2) -0.025(3) C24 0.140(6) 0.172(9) 0.073(3) 0.025(4) 0.013(3) -0.085(6) C25 0.109(4) 0.093(5) 0.083(4) -0.015(3) 0.020(3) -0.039(4) N51 0.063(2) 0.072(2) 0.048(2) -0.003(2) 0.016(1) 0.002(2) C51 0.067(2) 0.096(4) 0.048(2) -0.009(2) 0.009(2) 0.001(3) C52 0.059(2) 0.077(3) 0.062(2) -0.013(2) 0.005(2) -0.006(2) C53 0.058(2) 0.074(3) 0.069(3) -0.003(2) 0.018(2) -0.012(2) C54 0.055(2) 0.058(3) 0.055(2) -0.003(2) 0.015(2) -0.005(2) C55 0.053(2) 0.052(2) 0.045(2) -0.000(2) 0.014(1) 0.005(2) N52 0.044(1) 0.054(2) 0.048(2) -0.002(2) 0.009(1) 0.001(1) C56 0.049(2) 0.050(2) 0.047(2) 0.003(2) 0.014(1) 0.005(2) C57 0.054(2) 0.062(3) 0.051(2) 0.004(2) 0.016(2) 0.009(2) C58 0.052(2) 0.069(3) 0.062(2) 0.005(2) 0.024(2) -0.008(2) C59 0.049(2) 0.058(3) 0.057(2) -0.003(2) 0.012(2) -0.010(2) C60 0.045(2) 0.047(2) 0.050(2) -0.001(2) 0.014(1) 0.005(2) N53 0.050(1) 0.055(2) 0.047(2) -0.003(2) 0.014(1) -0.004(2) C61 0.044(2) 0.056(2) 0.046(2) -0.003(2) 0.011(1) -0.003(2) C62 0.048(2) 0.055(2) 0.059(2) -0.005(2) 0.018(2) -0.008(2) C63 0.060(2) 0.066(3) 0.062(2) 0.006(2) 0.027(2) -0.005(2) C64 0.062(2) 0.056(3) 0.051(2) -0.000(2) 0.021(2) 0.005(2) C65 0.050(2) 0.054(2) 0.048(2) -0.000(2) 0.011(1) 0.000(2) O51 0.066(2) 0.072(2) 0.043(1) -0.003(1) 0.015(1) -0.017(2) C66 0.056(2) 0.064(2) 0.045(2) 0.001(2) 0.014(2) -0.005(2) C67 0.053(2) 0.077(3) 0.057(2) 0.013(2) -0.002(2) -0.007(2) C68 0.066(2) 0.061(3) 0.074(3) 0.010(2) 0.008(2) 0.003(2) C69 0.080(3) 0.093(4) 0.086(3) -0.021(3) 0.029(3) 0.008(3) C70 0.073(2) 0.088(3) 0.047(2) -0.010(2) 0.019(2) -0.011(3) C71 0.046(2) 0.070(3) 0.047(2) -0.006(2) 0.005(1) 0.000(2) C72 0.063(3) 0.109(5) 0.095(4) 0.007(4) -0.002(2) 0.018(3) C73 0.056(2) 0.070(3) 0.056(2) -0.008(2) 0.014(2) -0.010(2) C74 0.090(3) 0.094(4) 0.083(3) -0.014(3) 0.042(3) -0.032(3) C75 0.081(3) 0.105(5) 0.082(3) -0.014(3) 0.017(3) -0.024(4) _refine_ls_extinction_coef 13.3(43) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 . C1 . 1.328(6) yes N1 . C5 . 1.347(5) yes C1 . C2 . 1.369(7) yes C1 . H11 . 0.960(4) no C2 . C3 . 1.383(6) yes C2 . H21 . 0.960(4) no C3 . C4 . 1.374(6) yes C3 . H31 . 0.960(4) no C4 . C5 . 1.380(6) yes C4 . H41 . 0.960(4) no C5 . C6 . 1.490(5) yes N2 . C6 . 1.334(5) yes N2 . C10 . 1.337(5) yes C6 . C7 . 1.398(5) yes C7 . C8 . 1.385(6) yes C7 . H71 . 0.960(4) no C8 . C9 . 1.379(6) yes C8 . H81 . 0.960(4) no C9 . C10 . 1.391(5) yes C9 . H91 . 0.960(4) no C10 . C11 . 1.491(5) yes N3 . C11 . 1.346(5) yes N3 . C15 . 1.312(5) yes C11 . C12 . 1.389(6) yes C12 . C13 . 1.382(6) yes C12 . H121 . 0.960(4) no C13 . C14 . 1.364(6) yes C13 . H131 . 0.960(4) no C14 . C15 . 1.401(6) yes C14 . H141 . 0.960(4) no C15 . O1 . 1.355(5) yes O1 . C16 . 1.456(5) yes C16 . C17 . 1.537(7) yes C16 . C21 . 1.510(6) yes C16 . H161 . 0.960(4) no C17 . C18 . 1.541(9) yes C17 . H171 . 0.960(9) no C17 . H172 . 0.960(8) no C18 . C19 . 1.52(1) yes C18 . C23 . 1.55(1) yes C18 . H181 . 0.960(5) no C19 . C20 . 1.49(1) yes C19 . H191 . 0.960(7) no C19 . H192 . 0.960(9) no C20 . C21 . 1.519(7) yes C20 . H201 . 0.960(6) no C20 . H202 . 0.960(6) no C21 . C22 . 1.513(8) yes C21 . C23 . 1.574(6) yes C22 . H221 . 0.960(7) no C22 . H222 . 0.960(7) no C22 . H223 . 0.960(8) no C23 . C24 . 1.498(8) yes C23 . C25 . 1.512(8) yes C24 . H241 . 0.960(7) no C24 . H242 . 0.96(1) no C24 . H243 . 0.960(7) no C25 . H251 . 0.960(6) no C25 . H252 . 0.960(8) no C25 . H253 . 0.960(6) no N51 . C51 . 1.330(6) yes N51 . C55 . 1.338(5) yes C51 . C52 . 1.375(7) yes C51 . H511 . 0.960(4) no C52 . C53 . 1.371(6) yes C52 . H521 . 0.960(4) no C53 . C54 . 1.376(6) yes C53 . H531 . 0.960(4) no C54 . C55 . 1.389(5) yes C54 . H541 . 0.960(4) no C55 . C56 . 1.485(6) yes N52 . C56 . 1.339(5) yes N52 . C60 . 1.343(5) yes C56 . C57 . 1.411(6) yes C57 . C58 . 1.365(6) yes C57 . H571 . 0.960(4) no C58 . C59 . 1.380(6) yes C58 . H581 . 0.960(4) no C59 . C60 . 1.393(5) yes C59 . H591 . 0.960(4) no C60 . C61 . 1.496(5) yes N53 . C61 . 1.350(5) yes N53 . C65 . 1.332(5) yes C61 . C62 . 1.389(6) yes C62 . C63 . 1.393(6) yes C62 . H621 . 0.960(4) no C63 . C64 . 1.366(6) yes C63 . H631 . 0.960(4) no C64 . C65 . 1.383(6) yes C64 . H641 . 0.960(4) no C65 . O51 . 1.363(5) yes O51 . C66 . 1.458(5) yes C66 . C67 . 1.516(6) yes C66 . C71 . 1.537(5) yes C66 . H661 . 0.960(4) no C67 . C68 . 1.546(7) yes C67 . H671 . 0.960(4) no C67 . H672 . 0.960(4) no C68 . C69 . 1.516(7) yes C68 . C73 . 1.553(6) yes C68 . H681 . 0.960(5) no C69 . C70 . 1.538(8) yes C69 . H691 . 0.960(6) no C69 . H692 . 0.960(6) no C70 . C71 . 1.531(6) yes C70 . H701 . 0.960(5) no C70 . H702 . 0.960(4) no C71 . C72 . 1.510(7) yes C71 . C73 . 1.548(7) yes C72 . H721 . 0.960(6) no C72 . H722 . 0.960(7) no C72 . H723 . 0.960(8) no C73 . C74 . 1.527(6) yes C73 . C75 . 1.539(8) yes C74 . H741 . 0.960(5) no C74 . H742 . 0.960(6) no C74 . H743 . 0.960(6) no C75 . H751 . 0.960(6) no C75 . H752 . 0.960(7) no C75 . H753 . 0.960(6) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . N1 . C5 . 117.2(4) no N1 . C1 . C2 . 124.9(4) no N1 . C1 . H11 . 117.6(4) no C2 . C1 . H11 . 117.6(4) no C1 . C2 . C3 . 117.4(4) no C1 . C2 . H21 . 121.3(5) no C3 . C2 . H21 . 121.3(5) no C2 . C3 . C4 . 119.1(4) no C2 . C3 . H31 . 120.4(4) no C4 . C3 . H31 . 120.4(4) no C3 . C4 . C5 . 119.6(4) no C3 . C4 . H41 . 120.2(4) no C5 . C4 . H41 . 120.2(4) no N1 . C5 . C4 . 121.8(4) no N1 . C5 . C6 . 116.2(3) no C4 . C5 . C6 . 122.0(3) no C6 . N2 . C10 . 118.4(3) no C5 . C6 . N2 . 116.4(3) no C5 . C6 . C7 . 121.0(3) no N2 . C6 . C7 . 122.7(4) no C6 . C7 . C8 . 118.5(4) no C6 . C7 . H71 . 120.8(4) no C8 . C7 . H71 . 120.8(4) no C7 . C8 . C9 . 119.0(4) no C7 . C8 . H81 . 120.5(4) no C9 . C8 . H81 . 120.5(4) no C8 . C9 . C10 . 119.0(4) no C8 . C9 . H91 . 120.5(4) no C10 . C9 . H91 . 120.5(4) no N2 . C10 . C9 . 122.5(3) no N2 . C10 . C11 . 116.3(3) no C9 . C10 . C11 . 121.2(3) no C11 . N3 . C15 . 117.8(3) no C10 . C11 . N3 . 116.1(3) no C10 . C11 . C12 . 121.6(4) no N3 . C11 . C12 . 122.3(3) no C11 . C12 . C13 . 118.3(4) no C11 . C12 . H121 . 120.9(4) no C13 . C12 . H121 . 120.9(4) no C12 . C13 . C14 . 120.3(4) no C12 . C13 . H131 . 119.8(4) no C14 . C13 . H131 . 119.8(4) no C13 . C14 . C15 . 117.0(3) no C13 . C14 . H141 . 121.5(4) no C15 . C14 . H141 . 121.5(4) no N3 . C15 . C14 . 124.3(4) no N3 . C15 . O1 . 119.6(4) no C14 . C15 . O1 . 116.1(3) no C15 . O1 . C16 . 116.2(3) no O1 . C16 . C17 . 113.0(5) no O1 . C16 . C21 . 109.5(3) no C17 . C16 . C21 . 104.0(4) no O1 . C16 . H161 . 103.0(3) no C17 . C16 . H161 . 112.7(4) no C21 . C16 . H161 . 114.7(5) no C16 . C17 . C18 . 102.4(4) no C16 . C17 . H171 . 111.2(5) no C18 . C17 . H171 . 111.2(7) no C16 . C17 . H172 . 111.2(7) no C18 . C17 . H172 . 111.2(6) no H171 . C17 . H172 . 109.5(6) no C17 . C18 . C19 . 106.9(6) no C17 . C18 . C23 . 102.9(5) no C19 . C18 . C23 . 102.1(6) no C17 . C18 . H181 . 113.1(6) no C19 . C18 . H181 . 112.9(7) no C23 . C18 . H181 . 117.7(7) no C18 . C19 . C20 . 103.5(5) no C18 . C19 . H191 . 110.9(8) no C20 . C19 . H191 . 111.0(9) no C18 . C19 . H192 . 110.9(9) no C20 . C19 . H192 . 110.9(8) no H191 . C19 . H192 . 109.5(6) no C19 . C20 . C21 . 105.0(5) no C19 . C20 . H201 . 110.6(6) no C21 . C20 . H201 . 110.6(7) no C19 . C20 . H202 . 110.6(8) no C21 . C20 . H202 . 110.6(4) no H201 . C20 . H202 . 109.5(6) no C16 . C21 . C20 . 108.5(5) no C16 . C21 . C22 . 112.9(4) no C20 . C21 . C22 . 114.5(5) no C16 . C21 . C23 . 101.2(3) no C20 . C21 . C23 . 101.4(4) no C22 . C21 . C23 . 116.8(5) no C21 . C22 . H221 . 109.5(6) no C21 . C22 . H222 . 109.5(6) no H221 . C22 . H222 . 109.5(6) no C21 . C22 . H223 . 109.5(5) no H221 . C22 . H223 . 109.5(7) no H222 . C22 . H223 . 109.5(7) no C18 . C23 . C21 . 91.3(4) no C18 . C23 . C24 . 114.0(6) no C21 . C23 . C24 . 113.9(4) no C18 . C23 . C25 . 112.9(5) no C21 . C23 . C25 . 116.3(4) no C24 . C23 . C25 . 107.9(6) no C23 . C24 . H241 . 109.5(7) no C23 . C24 . H242 . 109.5(6) no H241 . C24 . H242 . 109.5(8) no C23 . C24 . H243 . 109.5(6) no H241 . C24 . H243 . 109.5(8) no H242 . C24 . H243 . 109.5(8) no C23 . C25 . H251 . 109.5(6) no C23 . C25 . H252 . 109.5(5) no H251 . C25 . H252 . 109.5(6) no C23 . C25 . H253 . 109.5(6) no H251 . C25 . H253 . 109.5(6) no H252 . C25 . H253 . 109.5(7) no C51 . N51 . C55 . 117.8(4) no N51 . C51 . C52 . 123.2(4) no N51 . C51 . H511 . 118.4(5) no C52 . C51 . H511 . 118.4(5) no C51 . C52 . C53 . 119.0(4) no C51 . C52 . H521 . 120.5(5) no C53 . C52 . H521 . 120.5(5) no C52 . C53 . C54 . 118.9(4) no C52 . C53 . H531 . 120.6(4) no C54 . C53 . H531 . 120.6(4) no C53 . C54 . C55 . 118.8(4) no C53 . C54 . H541 . 120.6(4) no C55 . C54 . H541 . 120.6(4) no N51 . C55 . C54 . 122.3(4) no N51 . C55 . C56 . 117.0(3) no C54 . C55 . C56 . 120.7(3) no C56 . N52 . C60 . 118.4(3) no C55 . C56 . N52 . 116.9(3) no C55 . C56 . C57 . 121.1(3) no N52 . C56 . C57 . 122.0(4) no C56 . C57 . C58 . 118.5(4) no C56 . C57 . H571 . 120.8(4) no C58 . C57 . H571 . 120.8(4) no C57 . C58 . C59 . 120.2(4) no C57 . C58 . H581 . 119.9(4) no C59 . C58 . H581 . 119.9(4) no C58 . C59 . C60 . 118.3(4) no C58 . C59 . H591 . 120.8(4) no C60 . C59 . H591 . 120.8(4) no N52 . C60 . C59 . 122.6(3) no N52 . C60 . C61 . 116.9(3) no C59 . C60 . C61 . 120.5(3) no C61 . N53 . C65 . 116.8(3) no C60 . C61 . N53 . 116.4(3) no C60 . C61 . C62 . 120.8(3) no N53 . C61 . C62 . 122.9(3) no C61 . C62 . C63 . 118.0(4) no C61 . C62 . H621 . 121.0(4) no C63 . C62 . H621 . 121.0(4) no C62 . C63 . C64 . 119.9(4) no C62 . C63 . H631 . 120.1(5) no C64 . C63 . H631 . 120.1(4) no C63 . C64 . C65 . 117.7(3) no C63 . C64 . H641 . 121.1(4) no C65 . C64 . H641 . 121.1(4) no N53 . C65 . C64 . 124.6(4) no N53 . C65 . O51 . 118.4(3) no C64 . C65 . O51 . 116.9(3) no C65 . O51 . C66 . 117.3(3) no O51 . C66 . C67 . 112.4(3) no O51 . C66 . C71 . 110.0(3) no C67 . C66 . C71 . 105.0(4) no O51 . C66 . H661 . 103.4(4) no C67 . C66 . H661 . 111.5(4) no C71 . C66 . H661 . 114.8(4) no C66 . C67 . C68 . 102.8(3) no C66 . C67 . H671 . 111.1(5) no C68 . C67 . H671 . 111.1(4) no C66 . C67 . H672 . 111.1(4) no C68 . C67 . H672 . 111.1(5) no H671 . C67 . H672 . 109.5(4) no C67 . C68 . C69 . 107.2(4) no C67 . C68 . C73 . 101.3(4) no C69 . C68 . C73 . 103.1(4) no C67 . C68 . H681 . 114.4(4) no C69 . C68 . H681 . 111.5(5) no C73 . C68 . H681 . 118.1(5) no C68 . C69 . C70 . 102.9(4) no C68 . C69 . H691 . 111.1(5) no C70 . C69 . H691 . 111.1(6) no C68 . C69 . H692 . 111.1(6) no C70 . C69 . H692 . 111.1(5) no H691 . C69 . H692 . 109.5(5) no C69 . C70 . C71 . 104.4(4) no C69 . C70 . H701 . 110.7(4) no C71 . C70 . H701 . 110.7(5) no C69 . C70 . H702 . 110.7(5) no C71 . C70 . H702 . 110.7(4) no H701 . C70 . H702 . 109.5(4) no C66 . C71 . C70 . 107.3(3) no C66 . C71 . C72 . 114.2(4) no C70 . C71 . C72 . 113.8(4) no C66 . C71 . C73 . 99.9(3) no C70 . C71 . C73 . 101.7(4) no C72 . C71 . C73 . 118.2(4) no C71 . C72 . H721 . 109.5(7) no C71 . C72 . H722 . 109.5(5) no H721 . C72 . H722 . 109.5(6) no C71 . C72 . H723 . 109.5(5) no H721 . C72 . H723 . 109.5(6) no H722 . C72 . H723 . 109.5(8) no C68 . C73 . C71 . 93.4(3) no C68 . C73 . C74 . 114.8(4) no C71 . C73 . C74 . 114.9(4) no C68 . C73 . C75 . 112.6(5) no C71 . C73 . C75 . 115.1(4) no C74 . C73 . C75 . 106.0(4) no C73 . C74 . H741 . 109.5(4) no C73 . C74 . H742 . 109.5(5) no H741 . C74 . H742 . 109.5(5) no C73 . C74 . H743 . 109.5(5) no H741 . C74 . H743 . 109.5(6) no H742 . C74 . H743 . 109.5(5) no C73 . C75 . H751 . 109.5(5) no C73 . C75 . H752 . 109.5(5) no H751 . C75 . H752 . 109.5(7) no C73 . C75 . H753 . 109.5(6) no H751 . C75 . H753 . 109.5(6) no H752 . C75 . H753 . 109.5(6) no data_TKA38 _audit_creation_date 98-03-25 _audit_creation_method CRYSTALS #========================================================================== _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 13.190(2) _cell_angle_alpha 90 _cell_length_b 7.750(1) _cell_angle_beta 105.390(7) _cell_length_c 21.469(1) _cell_angle_gamma 90 _cell_volume 2116.1(4) _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,y+1/2,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0170 0.0090 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0290 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0470 0.0320 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C25 H27 N3 O ' _chemical_formula_moiety ' C25 H27 N3 O ' _chemical_compound_source ; ? ; _chemical_formula_weight 385.51 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 23 _cell_measurement_theta_max 43 _cell_measurement_temperature 293 _cell_formula_units_Z 4 _exptl_crystal_description ' needle ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.26 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_max 0.55 _exptl_crystal_density_diffrn 1.21 _exptl_crystal_density_meas ? _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.55 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '\y scan' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time 120 _diffrn_standards_interval_count ? _diffrn_standards_number 3 _diffrn_standards_decay_% 3.47 _diffrn_ambient_temperature 293 _diffrn_reflns_number 5028 _reflns_number_total 4274 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_observed 3496 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 74.33 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 9 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.31 _refine_diff_density_max 0.33 _refine_ls_number_reflns 3496 _refine_ls_number_parameters 524 _refine_ls_R_factor_obs 0.0544 _refine_ls_wR_factor_obs 0.0652 _refine_ls_goodness_of_fit_obs 0.7580 _refine_ls_shift/esd_max 0.117820 _refine_ls_abs_structure_details 'not determined' _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method 2\q/\w # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type N1 0.4591(2) 0.6333(5) -0.3207(1) 0.0621 1.0000 Uani C1 0.3781(3) 0.7092(6) -0.3628(2) 0.0686 1.0000 Uani C2 0.2886(3) 0.7657(6) -0.3475(2) 0.0696 1.0000 Uani C3 0.2835(3) 0.7461(6) -0.2849(2) 0.0696 1.0000 Uani C4 0.3663(3) 0.6707(6) -0.2404(1) 0.0618 1.0000 Uani C5 0.4526(2) 0.6140(5) -0.2601(1) 0.0524 1.0000 Uani N2 0.5421(2) 0.5239(4) -0.1523(1) 0.0522 1.0000 Uani C6 0.5438(2) 0.5296(5) -0.2142(1) 0.0513 1.0000 Uani C7 0.6262(2) 0.4581(5) -0.2354(1) 0.0591 1.0000 Uani C8 0.7086(3) 0.3823(6) -0.1908(2) 0.0643 1.0000 Uani C9 0.7084(2) 0.3791(5) -0.1267(2) 0.0597 1.0000 Uani C10 0.6228(2) 0.4506(5) -0.1090(1) 0.0530 1.0000 Uani N3 0.6843(2) 0.3408(4) -0.0005(1) 0.0538 1.0000 Uani C11 0.6172(2) 0.4481(5) -0.0408(1) 0.0527 1.0000 Uani C12 0.5458(3) 0.5508(5) -0.0204(2) 0.0650 1.0000 Uani C13 0.5460(3) 0.5428(6) 0.0441(2) 0.0671 1.0000 Uani C14 0.6131(3) 0.4357(5) 0.0853(1) 0.0613 1.0000 Uani C15 0.6807(2) 0.3353(5) 0.0599(1) 0.0531 1.0000 Uani O1 0.7454(2) 0.2258(4) 0.1014(1) 0.0629 1.0000 Uani C16 0.7979(2) 0.0962(6) 0.0731(1) 0.0619 1.0000 Uani C17 0.8981(4) 0.1612(8) 0.0569(3) 0.1149 1.0000 Uani C18 0.9826(3) 0.0375(9) 0.0960(3) 0.1134 1.0000 Uani C19 1.0030(4) 0.089(1) 0.1662(4) 0.1398 1.0000 Uani C20 0.9039(4) 0.0319(8) 0.1826(2) 0.0989 1.0000 Uani C21 0.8373(3) -0.0487(5) 0.1211(1) 0.0627 1.0000 Uani C22 0.9217(3) -0.1323(7) 0.0922(2) 0.0742 1.0000 Uani C23 0.8792(5) -0.204(1) 0.0249(2) 0.1271 1.0000 Uani C24 0.9861(4) -0.2761(8) 0.1318(2) 0.0984 1.0000 Uani C25 0.7498(4) -0.1624(8) 0.1310(3) 0.1102 1.0000 Uani N101 0.5618(2) 0.0045(5) -0.1782(1) 0.0652 1.0000 Uani C101 0.6455(3) -0.0686(7) -0.1383(2) 0.0738 1.0000 Uani C102 0.7308(3) -0.1281(6) -0.1571(2) 0.0726 1.0000 Uani C103 0.7295(3) -0.1131(6) -0.2207(2) 0.0721 1.0000 Uani C104 0.6446(2) -0.0375(5) -0.2636(2) 0.0597 1.0000 Uani C105 0.5624(2) 0.0208(5) -0.2402(1) 0.0525 1.0000 Uani N102 0.4648(2) 0.1083(4) -0.3470(1) 0.0525 1.0000 Uani C106 0.4690(2) 0.1051(5) -0.2839(1) 0.0521 1.0000 Uani C107 0.3894(2) 0.1768(5) -0.2601(1) 0.0575 1.0000 Uani C108 0.3053(2) 0.2528(6) -0.3021(2) 0.0620 1.0000 Uani C109 0.3002(2) 0.2568(5) -0.3676(2) 0.0588 1.0000 Uani C110 0.3816(2) 0.1826(5) -0.3880(1) 0.0508 1.0000 Uani N103 0.3080(2) 0.2824(4) -0.4970(1) 0.0542 1.0000 Uani C111 0.3794(2) 0.1783(5) -0.4577(1) 0.0515 1.0000 Uani C112 0.4464(2) 0.0755(5) -0.4806(2) 0.0592 1.0000 Uani C113 0.4397(3) 0.0766(6) -0.5464(2) 0.0640 1.0000 Uani C114 0.3687(3) 0.1824(5) -0.5865(1) 0.0591 1.0000 Uani C115 0.3034(2) 0.2819(5) -0.5596(1) 0.0534 1.0000 Uani O101 0.2325(2) 0.3852(4) -0.6003(1) 0.0657 1.0000 Uani C116 0.1748(2) 0.5073(5) -0.5716(1) 0.0565 1.0000 Uani C117 0.2420(3) 0.6558(6) -0.5374(2) 0.0720 1.0000 Uani C118 0.1862(3) 0.8158(6) -0.5724(2) 0.0746 1.0000 Uani C119 0.2077(4) 0.8185(7) -0.6388(2) 0.0919 1.0000 Uani C120 0.1401(3) 0.6697(6) -0.6741(2) 0.0741 1.0000 Uani C121 0.0880(2) 0.5946(5) -0.6244(1) 0.0599 1.0000 Uani C122 0.0699(3) 0.7602(6) -0.5881(2) 0.0650 1.0000 Uani C123 0.0302(4) 0.7280(8) -0.5283(2) 0.0948 1.0000 Uani C124 -0.0051(4) 0.8914(8) -0.6293(2) 0.0954 1.0000 Uani C125 -0.0054(3) 0.4811(9) -0.6531(2) 0.0998 1.0000 Uani H11 0.3827 0.7253 -0.4063 0.0660 1.0000 Uiso H21 0.2317 0.8171 -0.3796 0.0667 1.0000 Uiso H31 0.2227 0.7847 -0.2723 0.0698 1.0000 Uiso H41 0.3643 0.6575 -0.1963 0.0615 1.0000 Uiso H71 0.6253 0.4619 -0.2803 0.0599 1.0000 Uiso H81 0.7658 0.3318 -0.2042 0.0656 1.0000 Uiso H91 0.7659 0.3287 -0.0948 0.0596 1.0000 Uiso H121 0.4978 0.6249 -0.0501 0.0649 1.0000 Uiso H131 0.4984 0.6136 0.0597 0.0690 1.0000 Uiso H141 0.6141 0.4291 0.1301 0.0620 1.0000 Uiso H161 0.7432 0.0652 0.0354 0.0615 1.0000 Uiso H171 0.9132 0.2785 0.0707 0.1210 1.0000 Uiso H172 0.8921 0.1524 0.0115 0.1210 1.0000 Uiso H181 1.0460 0.0349 0.0821 0.1079 1.0000 Uiso H191 1.0635 0.0304 0.1925 0.1202 1.0000 Uiso H192 1.0128 0.2114 0.1715 0.1202 1.0000 Uiso H201 0.9196 -0.0512 0.2170 0.0892 1.0000 Uiso H202 0.8683 0.1288 0.1950 0.0892 1.0000 Uiso H231 0.8376 -0.1178 -0.0024 0.1195 1.0000 Uiso H232 0.9367 -0.2371 0.0078 0.1195 1.0000 Uiso H233 0.8363 -0.3033 0.0265 0.1195 1.0000 Uiso H241 1.0151 -0.2371 0.1754 0.0982 1.0000 Uiso H242 1.0420 -0.3081 0.1133 0.0982 1.0000 Uiso H243 0.9417 -0.3743 0.1320 0.0982 1.0000 Uiso H251 0.7789 -0.2514 0.1616 0.1138 1.0000 Uiso H252 0.7134 -0.2139 0.0906 0.1138 1.0000 Uiso H253 0.7015 -0.0940 0.1470 0.1138 1.0000 Uiso H1011 0.6463 -0.0805 -0.0937 0.0713 1.0000 Uiso H1021 0.7897 -0.1789 -0.1264 0.0700 1.0000 Uiso H1031 0.7876 -0.1551 -0.2355 0.0716 1.0000 Uiso H1041 0.6424 -0.0255 -0.3085 0.0597 1.0000 Uiso H1071 0.3939 0.1727 -0.2147 0.0583 1.0000 Uiso H1081 0.2501 0.3030 -0.2867 0.0636 1.0000 Uiso H1091 0.2417 0.3097 -0.3980 0.0590 1.0000 Uiso H1121 0.4972 0.0039 -0.4516 0.0599 1.0000 Uiso H1131 0.4846 0.0035 -0.5635 0.0671 1.0000 Uiso H1141 0.3639 0.1881 -0.6319 0.0604 1.0000 Uiso H1161 0.1509 0.4358 -0.5418 0.0554 1.0000 Uiso H1171 0.3124 0.6474 -0.5417 0.0673 1.0000 Uiso H1172 0.2438 0.6582 -0.4924 0.0673 1.0000 Uiso H1181 0.2057 0.9215 -0.5489 0.0730 1.0000 Uiso H1191 0.1863 0.9263 -0.6603 0.0944 1.0000 Uiso H1192 0.2808 0.7990 -0.6354 0.0944 1.0000 Uiso H1201 0.0880 0.7112 -0.7113 0.0722 1.0000 Uiso H1202 0.1830 0.5845 -0.6873 0.0722 1.0000 Uiso H1231 0.0752 0.6459 -0.5007 0.0994 1.0000 Uiso H1232 0.0308 0.8345 -0.5054 0.0994 1.0000 Uiso H1233 -0.0402 0.6836 -0.5414 0.0994 1.0000 Uiso H1241 0.0167 0.9158 -0.6677 0.0936 1.0000 Uiso H1242 -0.0041 0.9958 -0.6051 0.0936 1.0000 Uiso H1243 -0.0751 0.8449 -0.6412 0.0936 1.0000 Uiso H1251 -0.0559 0.5444 -0.6855 0.0925 1.0000 Uiso H1252 0.0172 0.3815 -0.6724 0.0925 1.0000 Uiso H1253 -0.0370 0.4452 -0.6198 0.0925 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.059(1) 0.083(2) 0.045(1) 0.001(1) 0.015(1) -0.004(2) C1 0.068(2) 0.089(3) 0.047(2) 0.002(2) 0.013(1) -0.003(2) C2 0.060(2) 0.082(3) 0.060(2) 0.005(2) 0.005(1) -0.001(2) C3 0.062(2) 0.079(3) 0.069(2) 0.001(2) 0.020(2) 0.009(2) C4 0.062(2) 0.073(2) 0.051(2) 0.003(2) 0.017(1) 0.005(2) C5 0.053(1) 0.057(2) 0.048(1) 0.000(1) 0.014(1) -0.007(1) N2 0.054(1) 0.055(2) 0.049(1) 0.004(1) 0.016(1) 0.004(1) C6 0.051(1) 0.053(2) 0.052(2) 0.003(1) 0.015(1) -0.006(1) C7 0.059(2) 0.070(2) 0.052(2) 0.000(2) 0.021(1) -0.003(2) C8 0.056(2) 0.074(2) 0.068(2) 0.001(2) 0.025(1) 0.005(2) C9 0.053(1) 0.069(2) 0.058(2) 0.010(2) 0.016(1) 0.004(2) C10 0.051(1) 0.055(2) 0.054(2) 0.005(2) 0.016(1) -0.000(1) N3 0.051(1) 0.062(2) 0.050(1) 0.006(1) 0.017(1) 0.003(1) C11 0.050(1) 0.057(2) 0.052(2) 0.004(2) 0.014(1) -0.001(1) C12 0.065(2) 0.071(3) 0.059(2) 0.007(2) 0.017(1) 0.014(2) C13 0.073(2) 0.069(2) 0.065(2) -0.001(2) 0.029(2) 0.012(2) C14 0.068(2) 0.066(2) 0.053(2) -0.002(2) 0.022(1) 0.001(2) C15 0.052(1) 0.060(2) 0.046(1) 0.005(1) 0.011(1) -0.002(1) O1 0.066(1) 0.076(2) 0.049(1) 0.007(1) 0.0185(9) 0.012(1) C16 0.056(1) 0.085(2) 0.049(2) 0.014(2) 0.021(1) 0.014(2) C17 0.093(3) 0.130(4) 0.147(4) 0.071(4) 0.076(3) 0.035(3) C18 0.059(2) 0.132(5) 0.160(5) 0.056(4) 0.049(3) 0.022(3) C19 0.076(3) 0.130(6) 0.177(6) -0.023(5) -0.031(3) 0.014(4) C20 0.107(3) 0.115(4) 0.057(2) -0.002(2) -0.007(2) 0.034(3) C21 0.067(2) 0.072(2) 0.053(2) 0.011(2) 0.021(1) 0.007(2) C22 0.069(2) 0.097(3) 0.060(2) 0.019(2) 0.022(2) 0.023(2) C23 0.132(4) 0.167(6) 0.077(3) -0.024(3) 0.020(3) 0.074(4) C24 0.104(3) 0.099(4) 0.092(3) 0.015(3) 0.025(3) 0.034(3) C25 0.113(4) 0.086(3) 0.151(4) 0.024(3) 0.070(3) 0.001(3) N101 0.067(2) 0.077(2) 0.052(1) 0.009(1) 0.016(1) -0.001(2) C101 0.079(2) 0.091(3) 0.051(2) 0.012(2) 0.015(2) 0.003(2) C102 0.068(2) 0.080(3) 0.063(2) 0.014(2) 0.005(2) 0.006(2) C103 0.062(2) 0.086(3) 0.069(2) 0.009(2) 0.018(2) 0.014(2) C104 0.059(2) 0.066(2) 0.054(2) 0.003(2) 0.016(1) 0.005(2) C105 0.053(1) 0.056(2) 0.049(2) 0.002(1) 0.016(1) -0.006(1) N102 0.049(1) 0.061(2) 0.048(1) 0.000(1) 0.014(1) -0.001(1) C106 0.051(1) 0.056(2) 0.052(2) -0.002(1) 0.017(1) -0.004(1) C107 0.060(2) 0.067(2) 0.050(2) 0.000(2) 0.021(1) 0.000(2) C108 0.057(2) 0.073(2) 0.061(2) 0.001(2) 0.026(1) 0.008(2) C109 0.052(1) 0.064(2) 0.062(2) 0.003(2) 0.017(1) 0.011(2) C110 0.049(1) 0.054(2) 0.051(2) 0.002(1) 0.016(1) -0.001(1) N103 0.053(1) 0.064(2) 0.047(1) 0.003(1) 0.016(1) 0.004(1) C111 0.048(1) 0.058(2) 0.050(1) 0.003(2) 0.016(1) -0.001(1) C112 0.056(2) 0.061(2) 0.064(2) 0.004(2) 0.020(1) 0.007(2) C113 0.065(2) 0.067(2) 0.070(2) -0.003(2) 0.034(2) 0.008(2) C114 0.065(2) 0.065(2) 0.053(2) -0.002(2) 0.024(1) -0.003(2) C115 0.053(1) 0.057(2) 0.051(2) -0.001(1) 0.014(1) -0.003(2) O101 0.072(1) 0.080(2) 0.046(1) 0.002(1) 0.018(1) 0.015(1) C116 0.056(2) 0.072(2) 0.042(1) 0.006(1) 0.014(1) 0.010(2) C117 0.056(2) 0.090(3) 0.060(2) -0.013(2) -0.001(1) 0.011(2) C118 0.070(2) 0.075(2) 0.074(2) -0.006(2) 0.011(2) -0.004(2) C119 0.087(3) 0.099(4) 0.098(3) 0.018(3) 0.039(2) -0.009(3) C120 0.079(2) 0.098(3) 0.049(2) 0.014(2) 0.022(1) 0.016(2) C121 0.051(1) 0.076(2) 0.049(1) 0.004(2) 0.007(1) -0.002(2) C122 0.061(2) 0.077(3) 0.057(2) 0.009(2) 0.016(1) 0.015(2) C123 0.101(3) 0.111(4) 0.088(2) 0.018(3) 0.051(2) 0.037(3) C124 0.081(2) 0.115(4) 0.088(3) 0.023(3) 0.019(2) 0.035(3) C125 0.063(2) 0.120(4) 0.104(3) -0.008(3) 0.001(2) -0.012(3) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 . C1 . 1.339(5) yes N1 . C5 . 1.335(4) yes C1 . C2 . 1.379(5) yes C1 . H11 . 0.960(3) no C2 . C3 . 1.370(5) yes C2 . H21 . 0.960(4) no C3 . C4 . 1.376(5) yes C3 . H31 . 0.960(4) no C4 . C5 . 1.387(5) yes C4 . H41 . 0.960(3) no C5 . C6 . 1.490(4) yes N2 . C6 . 1.336(4) yes N2 . C10 . 1.339(4) yes C6 . C7 . 1.400(5) yes C7 . C8 . 1.375(5) yes C7 . H71 . 0.960(3) no C8 . C9 . 1.376(4) yes C8 . H81 . 0.960(3) no C9 . C10 . 1.398(5) yes C9 . H91 . 0.960(3) no C10 . C11 . 1.486(4) yes N3 . C11 . 1.347(4) yes N3 . C15 . 1.311(4) yes C11 . C12 . 1.390(5) yes C12 . C13 . 1.385(5) yes C12 . H121 . 0.960(4) no C13 . C14 . 1.357(5) yes C13 . H131 . 0.960(3) no C14 . C15 . 1.399(5) yes C14 . H141 . 0.960(3) no C15 . O1 . 1.357(4) yes O1 . C16 . 1.442(4) yes C16 . C17 . 1.538(5) yes C16 . C21 . 1.520(5) yes C16 . H161 . 0.960(3) no C17 . C18 . 1.538(7) yes C17 . H171 . 0.960(7) no C17 . H172 . 0.960(6) no C18 . C19 . 1.513(9) yes C18 . C22 . 1.532(8) yes C18 . H181 . 0.960(4) no C19 . C20 . 1.507(9) yes C19 . H191 . 0.959(6) no C19 . H192 . 0.961(8) no C20 . C21 . 1.512(6) yes C20 . H201 . 0.960(5) no C20 . H202 . 0.960(5) no C21 . C22 . 1.553(5) yes C21 . C25 . 1.512(6) yes C22 . C23 . 1.511(6) yes C22 . C24 . 1.518(6) yes C23 . H231 . 0.960(6) no C23 . H232 . 0.960(5) no C23 . H233 . 0.959(9) no C24 . H241 . 0.960(5) no C24 . H242 . 0.960(5) no C24 . H243 . 0.960(6) no C25 . H251 . 0.960(6) no C25 . H252 . 0.959(7) no C25 . H253 . 0.960(6) no N101 . C101 . 1.330(5) yes N101 . C105 . 1.339(4) yes C101 . C102 . 1.371(6) yes C101 . H1011 . 0.960(3) no C102 . C103 . 1.368(5) yes C102 . H1021 . 0.960(4) no C103 . C104 . 1.378(5) yes C103 . H1031 . 0.960(4) no C104 . C105 . 1.387(4) yes C104 . H1041 . 0.960(3) no C105 . C106 . 1.488(5) yes N102 . C106 . 1.340(4) yes N102 . C110 . 1.341(4) yes C106 . C107 . 1.400(4) yes C107 . C108 . 1.364(5) yes C107 . H1071 . 0.960(3) no C108 . C109 . 1.390(4) yes C108 . H1081 . 0.960(3) no C109 . C110 . 1.387(4) yes C109 . H1091 . 0.960(3) no C110 . C111 . 1.490(4) yes N103 . C111 . 1.352(4) yes N103 . C115 . 1.328(4) yes C111 . C112 . 1.374(5) yes C112 . C113 . 1.393(5) yes C112 . H1121 . 0.960(3) no C113 . C114 . 1.365(5) yes C113 . H1131 . 0.960(3) no C114 . C115 . 1.391(5) yes C114 . H1141 . 0.960(3) no C115 . O101 . 1.360(4) yes O101 . C116 . 1.450(4) yes C116 . C117 . 1.518(5) yes C116 . C121 . 1.538(4) yes C116 . H1161 . 0.960(3) no C117 . C118 . 1.533(6) yes C117 . H1171 . 0.960(4) no C117 . H1172 . 0.960(4) no C118 . C119 . 1.525(6) yes C118 . C122 . 1.542(5) yes C118 . H1181 . 0.960(4) no C119 . C120 . 1.530(7) yes C119 . H1191 . 0.960(5) no C119 . H1192 . 0.960(5) no C120 . C121 . 1.530(5) yes C120 . H1201 . 0.960(3) no C120 . H1202 . 0.960(4) no C121 . C122 . 1.552(6) yes C121 . C125 . 1.506(6) yes C122 . C123 . 1.530(5) yes C122 . C124 . 1.527(6) yes C123 . H1231 . 0.960(5) no C123 . H1232 . 0.960(6) no C123 . H1233 . 0.960(5) no C124 . H1241 . 0.960(5) no C124 . H1242 . 0.960(6) no C124 . H1243 . 0.960(5) no C125 . H1251 . 0.960(5) no C125 . H1252 . 0.960(6) no C125 . H1253 . 0.960(6) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . N1 . C5 . 117.4(3) no N1 . C1 . C2 . 124.0(3) no N1 . C1 . H11 . 118.0(3) no C2 . C1 . H11 . 118.0(4) no C1 . C2 . C3 . 117.8(3) no C1 . C2 . H21 . 121.1(4) no C3 . C2 . H21 . 121.1(4) no C2 . C3 . C4 . 119.5(3) no C2 . C3 . H31 . 120.3(4) no C4 . C3 . H31 . 120.3(4) no C3 . C4 . C5 . 119.1(3) no C3 . C4 . H41 . 120.5(3) no C5 . C4 . H41 . 120.4(3) no N1 . C5 . C4 . 122.2(3) no N1 . C5 . C6 . 116.4(3) no C4 . C5 . C6 . 121.4(3) no C6 . N2 . C10 . 118.9(3) no C5 . C6 . N2 . 116.7(3) no C5 . C6 . C7 . 121.3(3) no N2 . C6 . C7 . 122.1(3) no C6 . C7 . C8 . 118.7(3) no C6 . C7 . H71 . 120.7(3) no C8 . C7 . H71 . 120.7(3) no C7 . C8 . C9 . 119.6(3) no C7 . C8 . H81 . 120.2(3) no C9 . C8 . H81 . 120.2(3) no C8 . C9 . C10 . 118.7(3) no C8 . C9 . H91 . 120.7(3) no C10 . C9 . H91 . 120.7(3) no N2 . C10 . C9 . 122.0(3) no N2 . C10 . C11 . 116.8(3) no C9 . C10 . C11 . 121.1(3) no C11 . N3 . C15 . 117.7(3) no C10 . C11 . N3 . 116.4(3) no C10 . C11 . C12 . 121.2(3) no N3 . C11 . C12 . 122.5(3) no C11 . C12 . C13 . 117.8(3) no C11 . C12 . H121 . 121.1(3) no C13 . C12 . H121 . 121.1(3) no C12 . C13 . C14 . 120.5(3) no C12 . C13 . H131 . 119.8(4) no C14 . C13 . H131 . 119.7(3) no C13 . C14 . C15 . 117.3(3) no C13 . C14 . H141 . 121.3(3) no C15 . C14 . H141 . 121.4(3) no N3 . C15 . C14 . 124.2(3) no N3 . C15 . O1 . 119.3(3) no C14 . C15 . O1 . 116.5(3) no C15 . O1 . C16 . 116.5(2) no O1 . C16 . C17 . 113.8(4) no O1 . C16 . C21 . 110.2(2) no C17 . C16 . C21 . 103.6(3) no O1 . C16 . H161 . 101.1(3) no C17 . C16 . H161 . 113.0(3) no C21 . C16 . H161 . 115.6(4) no C16 . C17 . C18 . 102.4(3) no C16 . C17 . H171 . 111.2(4) no C18 . C17 . H171 . 111.2(6) no C16 . C17 . H172 . 111.2(5) no C18 . C17 . H172 . 111.2(5) no H171 . C17 . H172 . 109.5(5) no C17 . C18 . C19 . 106.9(5) no C17 . C18 . C22 . 102.3(4) no C19 . C18 . C22 . 103.4(5) no C17 . C18 . H181 . 114.1(5) no C19 . C18 . H181 . 112.1(6) no C22 . C18 . H181 . 116.9(6) no C18 . C19 . C20 . 102.7(4) no C18 . C19 . H191 . 111.2(7) no C20 . C19 . H191 . 111.2(8) no C18 . C19 . H192 . 111.1(8) no C20 . C19 . H192 . 111.1(6) no H191 . C19 . H192 . 109.4(5) no C19 . C20 . C21 . 104.8(4) no C19 . C20 . H201 . 110.6(5) no C21 . C20 . H201 . 110.6(5) no C19 . C20 . H202 . 110.7(6) no C21 . C20 . H202 . 110.6(4) no H201 . C20 . H202 . 109.5(5) no C16 . C21 . C20 . 107.5(4) no C16 . C21 . C22 . 100.9(2) no C20 . C21 . C22 . 102.1(3) no C16 . C21 . C25 . 112.9(3) no C20 . C21 . C25 . 114.0(4) no C22 . C21 . C25 . 117.9(4) no C18 . C22 . C21 . 92.4(4) no C18 . C22 . C23 . 115.1(5) no C21 . C22 . C23 . 114.4(3) no C18 . C22 . C24 . 113.2(4) no C21 . C22 . C24 . 115.8(3) no C23 . C22 . C24 . 106.0(4) no C22 . C23 . H231 . 109.4(5) no C22 . C23 . H232 . 109.4(5) no H231 . C23 . H232 . 109.4(6) no C22 . C23 . H233 . 109.5(5) no H231 . C23 . H233 . 109.5(6) no H232 . C23 . H233 . 109.5(6) no C22 . C24 . H241 . 109.5(5) no C22 . C24 . H242 . 109.5(4) no H241 . C24 . H242 . 109.5(5) no C22 . C24 . H243 . 109.5(4) no H241 . C24 . H243 . 109.4(5) no H242 . C24 . H243 . 109.4(6) no C21 . C25 . H251 . 109.4(5) no C21 . C25 . H252 . 109.5(4) no H251 . C25 . H252 . 109.5(6) no C21 . C25 . H253 . 109.4(5) no H251 . C25 . H253 . 109.5(5) no H252 . C25 . H253 . 109.5(6) no C101 . N101 . C105 . 117.2(3) no N101 . C101 . C102 . 124.0(3) no N101 . C101 . H1011 . 118.0(4) no C102 . C101 . H1011 . 118.0(4) no C101 . C102 . C103 . 118.2(3) no C101 . C102 . H1021 . 120.9(4) no C103 . C102 . H1021 . 120.9(4) no C102 . C103 . C104 . 119.7(3) no C102 . C103 . H1031 . 120.1(4) no C104 . C103 . H1031 . 120.1(4) no C103 . C104 . C105 . 118.1(3) no C103 . C104 . H1041 . 121.0(3) no C105 . C104 . H1041 . 120.9(3) no N101 . C105 . C104 . 122.8(3) no N101 . C105 . C106 . 116.6(3) no C104 . C105 . C106 . 120.7(3) no C106 . N102 . C110 . 118.6(3) no C105 . C106 . N102 . 116.8(3) no C105 . C106 . C107 . 121.3(3) no N102 . C106 . C107 . 121.9(3) no C106 . C107 . C108 . 119.1(3) no C106 . C107 . H1071 . 120.5(3) no C108 . C107 . H1071 . 120.5(3) no C107 . C108 . C109 . 119.5(3) no C107 . C108 . H1081 . 120.3(3) no C109 . C108 . H1081 . 120.3(3) no C108 . C109 . C110 . 118.4(3) no C108 . C109 . H1091 . 120.8(3) no C110 . C109 . H1091 . 120.8(3) no N102 . C110 . C109 . 122.5(3) no N102 . C110 . C111 . 116.4(3) no C109 . C110 . C111 . 121.1(3) no C111 . N103 . C115 . 117.8(3) no C110 . C111 . N103 . 116.0(3) no C110 . C111 . C112 . 122.0(3) no N103 . C111 . C112 . 122.0(3) no C111 . C112 . C113 . 119.1(3) no C111 . C112 . H1121 . 120.5(3) no C113 . C112 . H1121 . 120.5(3) no C112 . C113 . C114 . 119.5(3) no C112 . C113 . H1131 . 120.3(4) no C114 . C113 . H1131 . 120.3(3) no C113 . C114 . C115 . 117.9(3) no C113 . C114 . H1141 . 121.1(3) no C115 . C114 . H1141 . 121.0(3) no N103 . C115 . C114 . 123.7(3) no N103 . C115 . O101 . 119.2(3) no C114 . C115 . O101 . 117.0(3) no C115 . O101 . C116 . 117.3(2) no O101 . C116 . C117 . 113.3(3) no O101 . C116 . C121 . 110.2(2) no C117 . C116 . C121 . 104.4(3) no O101 . C116 . H1161 . 102.1(3) no C117 . C116 . H1161 . 111.6(3) no C121 . C116 . H1161 . 115.6(3) no C116 . C117 . C118 . 103.5(2) no C116 . C117 . H1171 . 110.9(3) no C118 . C117 . H1171 . 110.9(4) no C116 . C117 . H1172 . 110.9(4) no C118 . C117 . H1172 . 110.9(4) no H1171 . C117 . H1172 . 109.5(3) no C117 . C118 . C119 . 106.6(4) no C117 . C118 . C122 . 101.6(3) no C119 . C118 . C122 . 102.7(3) no C117 . C118 . H1181 . 114.0(3) no C119 . C118 . H1181 . 112.8(4) no C122 . C118 . H1181 . 117.7(4) no C118 . C119 . C120 . 103.0(3) no C118 . C119 . H1191 . 111.1(5) no C120 . C119 . H1191 . 111.1(4) no C118 . C119 . H1192 . 111.1(4) no C120 . C119 . H1192 . 111.1(5) no H1191 . C119 . H1192 . 109.4(4) no C119 . C120 . C121 . 104.6(3) no C119 . C120 . H1201 . 110.7(4) no C121 . C120 . H1201 . 110.7(3) no C119 . C120 . H1202 . 110.7(4) no C121 . C120 . H1202 . 110.7(4) no H1201 . C120 . H1202 . 109.5(3) no C116 . C121 . C120 . 107.3(3) no C116 . C121 . C122 . 100.2(3) no C120 . C121 . C122 . 101.1(3) no C116 . C121 . C125 . 114.4(4) no C120 . C121 . C125 . 114.0(3) no C122 . C121 . C125 . 118.1(3) no C118 . C122 . C121 . 93.7(3) no C118 . C122 . C123 . 113.8(3) no C121 . C122 . C123 . 114.7(4) no C118 . C122 . C124 . 113.3(4) no C121 . C122 . C124 . 115.0(3) no C123 . C122 . C124 . 106.3(3) no C122 . C123 . H1231 . 109.4(3) no C122 . C123 . H1232 . 109.4(5) no H1231 . C123 . H1232 . 109.5(5) no C122 . C123 . H1233 . 109.5(4) no H1231 . C123 . H1233 . 109.5(6) no H1232 . C123 . H1233 . 109.5(4) no C122 . C124 . H1241 . 109.4(4) no C122 . C124 . H1242 . 109.5(4) no H1241 . C124 . H1242 . 109.5(6) no C122 . C124 . H1243 . 109.4(5) no H1241 . C124 . H1243 . 109.5(5) no H1242 . C124 . H1243 . 109.5(4) no C121 . C125 . H1251 . 109.4(5) no C121 . C125 . H1252 . 109.5(4) no H1251 . C125 . H1252 . 109.5(5) no C121 . C125 . H1253 . 109.5(4) no H1251 . C125 . H1253 . 109.5(5) no H1252 . C125 . H1253 . 109.5(6) no data_TKA57 _audit_creation_date 98-03-25 _audit_creation_method CRYSTALS #========================================================================== _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 6.929(2) _cell_angle_alpha 90 _cell_length_b 10.696(1) _cell_angle_beta 92.81(1) _cell_length_c 29.978(4) _cell_angle_gamma 90 _cell_volume 2219.0(6) _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,y+1/2,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0170 0.0090 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0290 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0470 0.0320 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'S ' 0.3190 0.5570 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C26 H29 N3 O ' _chemical_formula_moiety ' C26 H29 N3 O ' _chemical_compound_source ; ? ; _chemical_formula_weight 399.54 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 22 _cell_measurement_theta_max 42 _cell_measurement_temperature 293 _cell_formula_units_Z 2 _exptl_crystal_description ' cube ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.20 _exptl_crystal_density_meas ? _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.54 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '\y scan' _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time 120 _diffrn_standards_interval_count ? _diffrn_standards_number 3 _diffrn_standards_decay_% 4.04 _diffrn_ambient_temperature 293 _diffrn_reflns_number 4780 _reflns_number_total 4404 _diffrn_reflns_av_R_equivalents 0.01 _reflns_number_observed 3837 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 74.33 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _reflns_limit_h_min -8 _reflns_limit_h_max 8 _reflns_limit_k_min -13 _reflns_limit_k_max 0 _reflns_limit_l_min 0 _reflns_limit_l_max 37 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.20 _refine_diff_density_max 0.34 _refine_ls_number_reflns 3837 _refine_ls_number_parameters 542 _refine_ls_R_factor_obs 0.0469 _refine_ls_wR_factor_obs 0.0552 _refine_ls_goodness_of_fit_obs 0.8702 _refine_ls_shift/esd_max 0.025596 # _refine_ls_abs_structure_details # ' from Flack enantiopole 0.3(7): not reliable --> not refined further.' _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method 2\q/\w # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type O1 0.2337(3) 0.8077(2) 0.44591(6) 0.0479 1.0000 Uani N1 0.1889(3) 0.6323(2) 0.40146(7) 0.0413 1.0000 Uani C1 0.2964(4) 0.6954(2) 0.43094(8) 0.0409 1.0000 Uani C2 0.4755(4) 0.6547(3) 0.44907(9) 0.0486 1.0000 Uani C3 0.5416(4) 0.5414(3) 0.4345(1) 0.0537 1.0000 Uani C4 0.4328(4) 0.4732(3) 0.4036(1) 0.0511 1.0000 Uani C5 0.2567(4) 0.5208(3) 0.38787(8) 0.0406 1.0000 Uani N2 0.2081(3) 0.3575(2) 0.33321(7) 0.0435 1.0000 Uani C6 0.1262(4) 0.4490(2) 0.35615(8) 0.0413 1.0000 Uani C7 -0.0700(4) 0.4757(3) 0.35193(9) 0.0503 1.0000 Uani C8 -0.1866(4) 0.4045(3) 0.3239(1) 0.0545 1.0000 Uani C9 -0.1038(4) 0.3080(3) 0.30035(9) 0.0518 1.0000 Uani C10 0.0929(4) 0.2881(3) 0.30563(8) 0.0436 1.0000 Uani N3 0.0715(4) 0.1193(2) 0.25259(8) 0.0551 1.0000 Uani C11 0.1877(4) 0.1869(3) 0.28010(9) 0.0476 1.0000 Uani C12 0.3848(5) 0.1663(3) 0.2849(1) 0.0601 1.0000 Uani C13 0.4638(5) 0.0728(4) 0.2597(1) 0.0716 1.0000 Uani C14 0.3456(6) 0.0030(3) 0.2312(1) 0.0729 1.0000 Uani C15 0.1501(5) 0.0289(3) 0.2283(1) 0.0622 1.0000 Uani C16 0.0121(7) -0.0421(4) 0.1974(1) 0.0854 1.0000 Uani C17 0.0519(3) 0.8538(2) 0.42638(9) 0.0414 1.0000 Uani C18 0.0665(4) 0.9054(3) 0.37894(9) 0.0553 1.0000 Uani C19 -0.0057(4) 1.0405(3) 0.38288(9) 0.0532 1.0000 Uani C20 0.1548(5) 1.1141(3) 0.4082(1) 0.0665 1.0000 Uani C21 0.1507(4) 1.0616(3) 0.4555(1) 0.0542 1.0000 Uani C22 -0.0152(4) 0.9667(2) 0.45342(8) 0.0416 1.0000 Uani C23 -0.0926(5) 0.9324(3) 0.4981(1) 0.0638 1.0000 Uani C24 -0.1594(4) 1.0282(3) 0.41819(9) 0.0445 1.0000 Uani C25 -0.3320(4) 0.9471(3) 0.4029(1) 0.0622 1.0000 Uani C26 -0.2418(5) 1.1534(3) 0.4329(1) 0.0648 1.0000 Uani O31 0.2464(3) -0.1166(2) 0.06375(7) 0.0540 1.0000 Uani N31 0.3144(3) 0.0621(2) 0.10462(7) 0.0453 1.0000 Uani C31 0.2002(4) 0.0012(3) 0.07568(9) 0.0449 1.0000 Uani C32 0.0290(4) 0.0498(3) 0.05655(9) 0.0518 1.0000 Uani C33 -0.0238(4) 0.1672(3) 0.0695(1) 0.0584 1.0000 Uani C34 0.0926(4) 0.2330(3) 0.1001(1) 0.0527 1.0000 Uani C35 0.2621(4) 0.1780(3) 0.11660(9) 0.0451 1.0000 Uani N32 0.3216(3) 0.3389(2) 0.17144(7) 0.0454 1.0000 Uani C36 0.3979(4) 0.2448(3) 0.14807(9) 0.0467 1.0000 Uani C37 0.5916(4) 0.2128(3) 0.1524(1) 0.0531 1.0000 Uani C38 0.7134(4) 0.2818(3) 0.1807(1) 0.0557 1.0000 Uani C39 0.6369(4) 0.3791(3) 0.20423(9) 0.0502 1.0000 Uani C40 0.4390(4) 0.4038(3) 0.19938(9) 0.0452 1.0000 Uani N33 0.4669(4) 0.5720(3) 0.25258(8) 0.0537 1.0000 Uani C41 0.3476(4) 0.5042(3) 0.22568(9) 0.0470 1.0000 Uani C42 0.1500(4) 0.5246(3) 0.2220(1) 0.0560 1.0000 Uani C43 0.0731(5) 0.6181(4) 0.2476(1) 0.0671 1.0000 Uani C44 0.1947(6) 0.6877(4) 0.2751(1) 0.0686 1.0000 Uani C45 0.3906(5) 0.6630(3) 0.2772(1) 0.0594 1.0000 Uani C46 0.5281(6) 0.7335(4) 0.3077(1) 0.0808 1.0000 Uani C47 0.4146(4) -0.1730(3) 0.08598(9) 0.0470 1.0000 Uani C48 0.6068(5) -0.1241(3) 0.0706(1) 0.0683 1.0000 Uani C49 0.7029(5) -0.2429(4) 0.0537(2) 0.0806 1.0000 Uani C50 0.595(1) -0.2790(7) 0.0101(2) 0.1377 1.0000 Uani C51 0.4017(9) -0.3258(5) 0.0256(2) 0.1173 1.0000 Uani C52 0.4178(4) -0.3124(3) 0.0757(1) 0.0595 1.0000 Uani C53 0.2718(7) -0.3858(5) 0.1011(3) 0.1234 1.0000 Uani C54 0.6351(5) -0.3423(3) 0.0860(1) 0.0600 1.0000 Uani C55 0.7030(6) -0.3207(5) 0.1345(1) 0.0880 1.0000 Uani C56 0.6926(7) -0.4760(4) 0.0742(2) 0.0979 1.0000 Uani H21 0.5488 0.7037 0.4707 0.0484 1.0000 Uiso H31 0.6640 0.5098 0.4459 0.0532 1.0000 Uiso H41 0.4780 0.3941 0.3931 0.0510 1.0000 Uiso H71 -0.1231 0.5433 0.3685 0.0501 1.0000 Uiso H81 -0.3227 0.4209 0.3205 0.0539 1.0000 Uiso H91 -0.1823 0.2559 0.2807 0.0517 1.0000 Uiso H121 0.4646 0.2155 0.3052 0.0597 1.0000 Uiso H131 0.6002 0.0568 0.2621 0.0708 1.0000 Uiso H141 0.3981 -0.0627 0.2137 0.0721 1.0000 Uiso H161 0.0818 -0.1043 0.1817 0.0839 1.0000 Uiso H162 -0.0842 -0.0819 0.2145 0.0839 1.0000 Uiso H163 -0.0493 0.0148 0.1764 0.0839 1.0000 Uiso H171 -0.0282 0.7806 0.4269 0.0411 1.0000 Uiso H181 0.1976 0.9035 0.3700 0.0549 1.0000 Uiso H182 -0.0141 0.8588 0.3580 0.0549 1.0000 Uiso H191 -0.0450 1.0773 0.3547 0.0530 1.0000 Uiso H201 0.1275 1.2021 0.4077 0.0652 1.0000 Uiso H202 0.2777 1.0994 0.3957 0.0652 1.0000 Uiso H211 0.1264 1.1268 0.4765 0.0529 1.0000 Uiso H212 0.2709 1.0213 0.4639 0.0529 1.0000 Uiso H231 -0.1316 1.0070 0.5131 0.0626 1.0000 Uiso H232 0.0064 0.8908 0.5160 0.0626 1.0000 Uiso H233 -0.2018 0.8778 0.4936 0.0626 1.0000 Uiso H251 -0.2868 0.8671 0.3932 0.0601 1.0000 Uiso H252 -0.4153 0.9358 0.4272 0.0601 1.0000 Uiso H253 -0.4023 0.9874 0.3785 0.0601 1.0000 Uiso H261 -0.1379 1.2075 0.4429 0.0634 1.0000 Uiso H262 -0.3260 1.1397 0.4569 0.0634 1.0000 Uiso H263 -0.3131 1.1914 0.4082 0.0634 1.0000 Uiso H321 -0.0488 0.0029 0.0351 0.0513 1.0000 Uiso H331 -0.1415 0.2038 0.0574 0.0572 1.0000 Uiso H341 0.0565 0.3150 0.1097 0.0523 1.0000 Uiso H371 0.6404 0.1435 0.1361 0.0530 1.0000 Uiso H381 0.8487 0.2625 0.1838 0.0547 1.0000 Uiso H391 0.7188 0.4293 0.2238 0.0500 1.0000 Uiso H421 0.0685 0.4749 0.2022 0.0561 1.0000 Uiso H431 -0.0635 0.6339 0.2461 0.0674 1.0000 Uiso H441 0.1439 0.7536 0.2928 0.0679 1.0000 Uiso H461 0.4587 0.7957 0.3235 0.0796 1.0000 Uiso H462 0.5899 0.6767 0.3287 0.0796 1.0000 Uiso H463 0.6240 0.7733 0.2906 0.0796 1.0000 Uiso H471 0.3972 -0.1512 0.1166 0.0469 1.0000 Uiso H481 0.6822 -0.0874 0.0949 0.0652 1.0000 Uiso H482 0.5876 -0.0637 0.0471 0.0652 1.0000 Uiso H491 0.8397 -0.2345 0.0508 0.0803 1.0000 Uiso H501 0.6625 -0.3438 -0.0050 0.1235 1.0000 Uiso H502 0.5784 -0.2081 -0.0093 0.1235 1.0000 Uiso H511 0.3815 -0.4117 0.0172 0.1134 1.0000 Uiso H512 0.2975 -0.2758 0.0131 0.1134 1.0000 Uiso H531 0.2798 -0.4727 0.0935 0.1038 1.0000 Uiso H532 0.2991 -0.3757 0.1326 0.1038 1.0000 Uiso H533 0.1441 -0.3554 0.0934 0.1038 1.0000 Uiso H551 0.6694 -0.2374 0.1432 0.0869 1.0000 Uiso H552 0.8406 -0.3311 0.1376 0.0869 1.0000 Uiso H553 0.6416 -0.3800 0.1532 0.0869 1.0000 Uiso H561 0.6522 -0.4933 0.0437 0.0893 1.0000 Uiso H562 0.8304 -0.4848 0.0779 0.0893 1.0000 Uiso H563 0.6314 -0.5337 0.0935 0.0893 1.0000 Uiso 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 O1 0.048(1) 0.040(1) 0.055(1) -0.0083(8) -0.0043(8) 0.0064(8) N1 0.045(1) 0.035(1) 0.043(1) -0.0004(9) 0.0008(9) 0.0031(9) C1 0.044(1) 0.037(1) 0.042(1) 0.001(1) 0.002(1) 0.003(1) C2 0.046(1) 0.050(2) 0.050(1) 0.000(1) -0.001(1) 0.002(1) C3 0.046(1) 0.059(2) 0.055(1) -0.001(1) -0.003(1) 0.012(1) C4 0.051(1) 0.048(2) 0.054(1) -0.004(1) 0.002(1) 0.016(1) C5 0.043(1) 0.039(1) 0.041(1) 0.001(1) 0.004(1) 0.003(1) N2 0.048(1) 0.038(1) 0.045(1) -0.0002(9) 0.0033(9) 0.0017(9) C6 0.045(1) 0.036(1) 0.043(1) 0.003(1) 0.005(1) 0.004(1) C7 0.049(1) 0.046(2) 0.056(1) -0.005(1) 0.002(1) 0.006(1) C8 0.044(1) 0.056(2) 0.063(2) -0.002(1) -0.000(1) 0.004(1) C9 0.053(1) 0.051(2) 0.051(1) -0.004(1) -0.002(1) -0.004(1) C10 0.053(1) 0.036(1) 0.041(1) 0.003(1) 0.003(1) -0.001(1) N3 0.067(2) 0.045(1) 0.053(1) -0.007(1) 0.002(1) -0.002(1) C11 0.060(2) 0.039(1) 0.045(1) 0.003(1) 0.007(1) -0.002(1) C12 0.059(2) 0.051(2) 0.070(2) -0.012(2) 0.006(1) 0.001(1) C13 0.061(2) 0.063(2) 0.092(3) -0.017(2) 0.017(2) 0.005(2) C14 0.088(2) 0.055(2) 0.077(2) -0.018(2) 0.020(2) 0.003(2) C15 0.083(2) 0.049(2) 0.055(2) -0.008(1) 0.005(2) -0.005(2) C16 0.106(3) 0.074(2) 0.076(2) -0.026(2) -0.004(2) 0.001(2) C17 0.040(1) 0.036(1) 0.048(1) -0.006(1) 0.002(1) 0.003(1) C18 0.055(2) 0.066(2) 0.045(1) -0.005(1) 0.008(1) 0.015(1) C19 0.055(1) 0.059(2) 0.046(1) 0.012(1) 0.006(1) 0.007(1) C20 0.061(2) 0.053(2) 0.086(2) 0.018(2) 0.007(2) -0.008(1) C21 0.054(1) 0.041(1) 0.066(2) -0.004(1) -0.008(1) -0.002(1) C22 0.048(1) 0.034(1) 0.043(1) -0.003(1) 0.003(1) 0.002(1) C23 0.085(2) 0.057(2) 0.050(2) 0.001(1) 0.015(1) 0.011(2) C24 0.046(1) 0.038(1) 0.049(1) -0.001(1) 0.003(1) 0.005(1) C25 0.045(1) 0.060(2) 0.082(2) -0.006(2) -0.007(1) 0.006(1) C26 0.062(2) 0.050(2) 0.082(2) -0.006(2) -0.000(2) 0.014(2) O31 0.050(1) 0.049(1) 0.061(1) -0.0122(9) -0.0104(8) 0.0025(9) N31 0.043(1) 0.045(1) 0.049(1) -0.004(1) 0.0004(9) 0.001(1) C31 0.043(1) 0.046(2) 0.047(1) -0.000(1) 0.004(1) -0.003(1) C32 0.045(1) 0.058(2) 0.052(1) -0.003(1) -0.005(1) -0.005(1) C33 0.045(1) 0.064(2) 0.065(2) -0.002(2) -0.009(1) 0.010(1) C34 0.049(1) 0.049(2) 0.059(2) -0.006(1) -0.002(1) 0.007(1) C35 0.045(1) 0.047(1) 0.042(1) -0.002(1) 0.002(1) 0.001(1) N32 0.048(1) 0.044(1) 0.044(1) -0.001(1) 0.0018(9) 0.002(1) C36 0.049(1) 0.044(1) 0.047(1) 0.000(1) 0.002(1) 0.002(1) C37 0.050(1) 0.052(2) 0.058(2) -0.008(1) 0.001(1) 0.006(1) C38 0.043(1) 0.063(2) 0.061(2) -0.009(1) -0.001(1) 0.004(1) C39 0.051(1) 0.050(2) 0.050(1) -0.004(1) -0.005(1) -0.003(1) C40 0.050(1) 0.042(1) 0.043(1) 0.000(1) 0.003(1) 0.001(1) N33 0.063(1) 0.052(1) 0.046(1) -0.007(1) -0.001(1) -0.000(1) C41 0.056(1) 0.042(1) 0.044(1) 0.001(1) 0.004(1) -0.001(1) C42 0.055(2) 0.057(2) 0.056(2) -0.007(1) 0.007(1) -0.000(1) C43 0.065(2) 0.070(2) 0.067(2) -0.012(2) 0.013(2) 0.007(2) C44 0.086(2) 0.062(2) 0.058(2) -0.012(2) 0.013(2) 0.014(2) C45 0.078(2) 0.050(2) 0.050(1) -0.008(1) 0.003(1) -0.000(2) C46 0.096(3) 0.072(2) 0.073(2) -0.026(2) -0.011(2) -0.001(2) C47 0.045(1) 0.047(1) 0.049(1) -0.007(1) -0.001(1) -0.000(1) C48 0.054(2) 0.051(2) 0.100(3) 0.016(2) 0.010(2) -0.000(1) C49 0.069(2) 0.073(2) 0.104(3) 0.019(2) 0.036(2) 0.018(2) C50 0.205(7) 0.151(6) 0.061(3) 0.001(3) 0.039(3) 0.092(5) C51 0.145(4) 0.102(4) 0.098(3) -0.060(3) -0.056(3) 0.065(3) C52 0.051(2) 0.046(2) 0.081(2) -0.004(1) -0.009(1) -0.002(1) C53 0.065(2) 0.075(3) 0.231(7) 0.045(4) 0.007(3) -0.013(2) C54 0.050(2) 0.049(2) 0.081(2) 0.004(2) -0.003(1) 0.000(1) C55 0.080(2) 0.089(3) 0.092(3) 0.017(2) -0.024(2) 0.009(2) C56 0.084(3) 0.056(2) 0.152(4) -0.010(3) -0.013(3) 0.016(2) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 . C1 . 1.361(3) yes O1 . C17 . 1.449(3) yes N1 . C1 . 1.314(3) yes N1 . C5 . 1.352(3) yes C1 . C2 . 1.400(4) yes C2 . C3 . 1.375(4) yes C2 . H21 . 0.960(3) no C3 . C4 . 1.375(4) yes C3 . H31 . 0.960(3) no C4 . C5 . 1.383(4) yes C4 . H41 . 0.960(3) no C5 . C6 . 1.493(4) yes N2 . C6 . 1.338(3) yes N2 . C10 . 1.343(3) yes C6 . C7 . 1.389(4) yes C7 . C8 . 1.368(4) yes C7 . H71 . 0.960(3) no C8 . C9 . 1.390(4) yes C8 . H81 . 0.960(3) no C9 . C10 . 1.381(4) yes C9 . H91 . 0.960(3) no C10 . C11 . 1.496(4) yes N3 . C11 . 1.337(4) yes N3 . C15 . 1.341(4) yes C11 . C12 . 1.384(4) yes C12 . C13 . 1.382(5) yes C12 . H121 . 0.960(3) no C13 . C14 . 1.374(5) yes C13 . H131 . 0.960(4) no C14 . C15 . 1.382(5) yes C14 . H141 . 0.960(3) no C15 . C16 . 1.503(5) yes C16 . H161 . 0.960(4) no C16 . H162 . 0.960(5) no C16 . H163 . 0.960(5) no C17 . C18 . 1.534(4) yes C17 . C22 . 1.538(3) yes C17 . H171 . 0.960(3) no C18 . C19 . 1.536(4) yes C18 . H181 . 0.960(3) no C18 . H182 . 0.960(3) no C19 . C20 . 1.532(5) yes C19 . C24 . 1.543(4) yes C19 . H191 . 0.960(3) no C20 . C21 . 1.529(5) yes C20 . H201 . 0.960(4) no C20 . H202 . 0.960(4) no C21 . C22 . 1.533(4) yes C21 . H211 . 0.960(3) no C21 . H212 . 0.960(3) no C22 . C23 . 1.512(4) yes C22 . C24 . 1.563(4) yes C23 . H231 . 0.960(3) no C23 . H232 . 0.960(3) no C23 . H233 . 0.960(4) no C24 . C25 . 1.530(4) yes C24 . C26 . 1.529(4) yes C25 . H251 . 0.960(3) no C25 . H252 . 0.960(3) no C25 . H253 . 0.960(3) no C26 . H261 . 0.960(4) no C26 . H262 . 0.960(4) no C26 . H263 . 0.960(3) no O31 . C31 . 1.353(3) yes O31 . C47 . 1.446(3) yes N31 . C31 . 1.317(3) yes N31 . C35 . 1.345(4) yes C31 . C32 . 1.392(4) yes C32 . C33 . 1.370(5) yes C32 . H321 . 0.960(3) no C33 . C34 . 1.384(4) yes C33 . H331 . 0.960(3) no C34 . C35 . 1.383(4) yes C34 . H341 . 0.960(3) no C35 . C36 . 1.483(4) yes N32 . C36 . 1.349(4) yes N32 . C40 . 1.334(3) yes C36 . C37 . 1.385(4) yes C37 . C38 . 1.380(4) yes C37 . H371 . 0.960(3) no C38 . C39 . 1.378(4) yes C38 . H381 . 0.960(3) no C39 . C40 . 1.397(4) yes C39 . H391 . 0.960(3) no C40 . C41 . 1.492(4) yes N33 . C41 . 1.339(4) yes N33 . C45 . 1.345(4) yes C41 . C42 . 1.385(4) yes C42 . C43 . 1.382(5) yes C42 . H421 . 0.960(3) no C43 . C44 . 1.370(5) yes C43 . H431 . 0.960(4) no C44 . C45 . 1.382(5) yes C44 . H441 . 0.960(3) no C45 . C46 . 1.492(5) yes C46 . H461 . 0.960(4) no C46 . H462 . 0.960(4) no C46 . H463 . 0.960(5) no C47 . C48 . 1.523(4) yes C47 . C52 . 1.523(4) yes C47 . H471 . 0.960(3) no C48 . C49 . 1.533(5) yes C48 . H481 . 0.960(4) no C48 . H482 . 0.960(3) no C49 . C50 . 1.521(8) yes C49 . C54 . 1.529(5) yes C49 . H491 . 0.960(4) no C50 . C51 . 1.53(1) yes C50 . H501 . 0.960(5) no C50 . H502 . 0.960(6) no C51 . C52 . 1.507(6) yes C51 . H511 . 0.960(5) no C51 . H512 . 0.960(4) no C52 . C53 . 1.516(6) yes C52 . C54 . 1.556(4) yes C53 . H531 . 0.960(6) no C53 . H532 . 0.960(8) no C53 . H533 . 0.960(5) no C54 . C55 . 1.523(5) yes C54 . C56 . 1.531(5) yes C55 . H551 . 0.960(5) no C55 . H552 . 0.960(4) no C55 . H553 . 0.960(5) no C56 . H561 . 0.960(6) no C56 . H562 . 0.960(4) no C56 . H563 . 0.960(6) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . O1 . C17 . 116.9(2) no C1 . N1 . C5 . 117.5(2) no O1 . C1 . N1 . 119.7(2) no O1 . C1 . C2 . 116.0(2) no N1 . C1 . C2 . 124.3(2) no C1 . C2 . C3 . 117.0(3) no C1 . C2 . H21 . 121.5(3) no C3 . C2 . H21 . 121.5(3) no C2 . C3 . C4 . 120.1(3) no C2 . C3 . H31 . 120.0(3) no C4 . C3 . H31 . 119.9(3) no C3 . C4 . C5 . 118.7(3) no C3 . C4 . H41 . 120.7(3) no C5 . C4 . H41 . 120.7(3) no N1 . C5 . C4 . 122.4(2) no N1 . C5 . C6 . 116.0(2) no C4 . C5 . C6 . 121.6(2) no C6 . N2 . C10 . 117.8(2) no C5 . C6 . N2 . 116.4(2) no C5 . C6 . C7 . 120.8(2) no N2 . C6 . C7 . 122.8(2) no C6 . C7 . C8 . 119.1(3) no C6 . C7 . H71 . 120.4(3) no C8 . C7 . H71 . 120.4(3) no C7 . C8 . C9 . 118.6(3) no C7 . C8 . H81 . 120.7(3) no C9 . C8 . H81 . 120.7(3) no C8 . C9 . C10 . 119.0(3) no C8 . C9 . H91 . 120.5(3) no C10 . C9 . H91 . 120.5(3) no N2 . C10 . C9 . 122.6(2) no N2 . C10 . C11 . 116.9(2) no C9 . C10 . C11 . 120.5(2) no C11 . N3 . C15 . 118.4(3) no C10 . C11 . N3 . 116.2(3) no C10 . C11 . C12 . 121.2(3) no N3 . C11 . C12 . 122.6(3) no C11 . C12 . C13 . 118.3(3) no C11 . C12 . H121 . 120.9(3) no C13 . C12 . H121 . 120.9(3) no C12 . C13 . C14 . 119.5(3) no C12 . C13 . H131 . 120.2(4) no C14 . C13 . H131 . 120.2(4) no C13 . C14 . C15 . 118.8(3) no C13 . C14 . H141 . 120.6(4) no C15 . C14 . H141 . 120.6(4) no N3 . C15 . C14 . 122.2(3) no N3 . C15 . C16 . 115.8(3) no C14 . C15 . C16 . 122.0(3) no C15 . C16 . H161 . 109.5(4) no C15 . C16 . H162 . 109.5(3) no H161 . C16 . H162 . 109.5(5) no C15 . C16 . H163 . 109.5(4) no H161 . C16 . H163 . 109.5(4) no H162 . C16 . H163 . 109.5(4) no O1 . C17 . C18 . 113.7(2) no O1 . C17 . C22 . 109.5(2) no C18 . C17 . C22 . 104.0(2) no O1 . C17 . H171 . 102.0(2) no C18 . C17 . H171 . 111.9(2) no C22 . C17 . H171 . 116.2(2) no C17 . C18 . C19 . 103.3(2) no C17 . C18 . H181 . 111.0(3) no C19 . C18 . H181 . 111.0(3) no C17 . C18 . H182 . 111.0(3) no C19 . C18 . H182 . 111.0(3) no H181 . C18 . H182 . 109.5(3) no C18 . C19 . C20 . 106.9(3) no C18 . C19 . C24 . 102.2(2) no C20 . C19 . C24 . 102.3(2) no C18 . C19 . H191 . 113.4(3) no C20 . C19 . H191 . 113.1(3) no C24 . C19 . H191 . 117.6(3) no C19 . C20 . C21 . 103.0(2) no C19 . C20 . H201 . 111.1(3) no C21 . C20 . H201 . 111.1(3) no C19 . C20 . H202 . 111.1(3) no C21 . C20 . H202 . 111.1(3) no H201 . C20 . H202 . 109.5(3) no C20 . C21 . C22 . 104.6(2) no C20 . C21 . H211 . 110.7(3) no C22 . C21 . H211 . 110.7(3) no C20 . C21 . H212 . 110.7(3) no C22 . C21 . H212 . 110.7(3) no H211 . C21 . H212 . 109.5(3) no C17 . C22 . C21 . 107.2(2) no C17 . C22 . C23 . 114.0(2) no C21 . C22 . C23 . 114.9(2) no C17 . C22 . C24 . 100.0(2) no C21 . C22 . C24 . 101.7(2) no C23 . C22 . C24 . 117.3(2) no C22 . C23 . H231 . 109.5(3) no C22 . C23 . H232 . 109.5(3) no H231 . C23 . H232 . 109.5(3) no C22 . C23 . H233 . 109.5(3) no H231 . C23 . H233 . 109.5(3) no H232 . C23 . H233 . 109.5(3) no C19 . C24 . C22 . 93.4(2) no C19 . C24 . C25 . 113.5(2) no C22 . C24 . C25 . 115.4(2) no C19 . C24 . C26 . 113.8(3) no C22 . C24 . C26 . 114.1(2) no C25 . C24 . C26 . 106.6(2) no C24 . C25 . H251 . 109.5(2) no C24 . C25 . H252 . 109.5(3) no H251 . C25 . H252 . 109.5(4) no C24 . C25 . H253 . 109.5(3) no H251 . C25 . H253 . 109.5(3) no H252 . C25 . H253 . 109.5(3) no C24 . C26 . H261 . 109.5(3) no C24 . C26 . H262 . 109.5(3) no H261 . C26 . H262 . 109.5(3) no C24 . C26 . H263 . 109.5(3) no H261 . C26 . H263 . 109.5(4) no H262 . C26 . H263 . 109.5(3) no C31 . O31 . C47 . 117.5(2) no C31 . N31 . C35 . 118.0(2) no O31 . C31 . N31 . 119.5(2) no O31 . C31 . C32 . 116.5(2) no N31 . C31 . C32 . 124.0(3) no C31 . C32 . C33 . 117.3(3) no C31 . C32 . H321 . 121.3(3) no C33 . C32 . H321 . 121.3(3) no C32 . C33 . C34 . 120.0(3) no C32 . C33 . H331 . 120.0(3) no C34 . C33 . H331 . 120.0(3) no C33 . C34 . C35 . 118.5(3) no C33 . C34 . H341 . 120.8(3) no C35 . C34 . H341 . 120.8(3) no N31 . C35 . C34 . 122.2(3) no N31 . C35 . C36 . 116.3(2) no C34 . C35 . C36 . 121.5(3) no C36 . N32 . C40 . 118.1(2) no C35 . C36 . N32 . 115.9(2) no C35 . C36 . C37 . 121.5(3) no N32 . C36 . C37 . 122.5(2) no C36 . C37 . C38 . 119.1(3) no C36 . C37 . H371 . 120.4(3) no C38 . C37 . H371 . 120.4(3) no C37 . C38 . C39 . 118.6(2) no C37 . C38 . H381 . 120.7(3) no C39 . C38 . H381 . 120.7(3) no C38 . C39 . C40 . 119.4(2) no C38 . C39 . H391 . 120.3(3) no C40 . C39 . H391 . 120.3(3) no N32 . C40 . C39 . 122.2(3) no N32 . C40 . C41 . 116.4(2) no C39 . C40 . C41 . 121.4(2) no C41 . N33 . C45 . 118.3(3) no C40 . C41 . N33 . 116.3(3) no C40 . C41 . C42 . 121.0(3) no N33 . C41 . C42 . 122.8(3) no C41 . C42 . C43 . 118.4(3) no C41 . C42 . H421 . 120.8(3) no C43 . C42 . H421 . 120.8(3) no C42 . C43 . C44 . 119.0(3) no C42 . C43 . H431 . 120.5(4) no C44 . C43 . H431 . 120.5(4) no C43 . C44 . C45 . 119.8(3) no C43 . C44 . H441 . 120.1(4) no C45 . C44 . H441 . 120.1(4) no N33 . C45 . C44 . 121.7(3) no N33 . C45 . C46 . 116.5(3) no C44 . C45 . C46 . 121.8(3) no C45 . C46 . H461 . 109.5(4) no C45 . C46 . H462 . 109.5(4) no H461 . C46 . H462 . 109.5(4) no C45 . C46 . H463 . 109.5(3) no H461 . C46 . H463 . 109.5(4) no H462 . C46 . H463 . 109.5(4) no O31 . C47 . C48 . 114.5(3) no O31 . C47 . C52 . 109.5(2) no C48 . C47 . C52 . 104.6(3) no O31 . C47 . H471 . 101.7(2) no C48 . C47 . H471 . 111.0(3) no C52 . C47 . H471 . 115.8(3) no C47 . C48 . C49 . 102.5(3) no C47 . C48 . H481 . 111.2(3) no C49 . C48 . H481 . 111.2(3) no C47 . C48 . H482 . 111.2(3) no C49 . C48 . H482 . 111.2(4) no H481 . C48 . H482 . 109.5(3) no C48 . C49 . C50 . 107.0(4) no C48 . C49 . C54 . 102.4(3) no C50 . C49 . C54 . 102.4(4) no C48 . C49 . H491 . 113.5(4) no C50 . C49 . H491 . 113.0(4) no C54 . C49 . H491 . 117.3(4) no C49 . C50 . C51 . 102.9(3) no C49 . C50 . H501 . 111.1(6) no C51 . C50 . H501 . 111.1(7) no C49 . C50 . H502 . 111.1(7) no C51 . C50 . H502 . 111.1(6) no H501 . C50 . H502 . 109.5(5) no C50 . C51 . C52 . 104.4(4) no C50 . C51 . H511 . 110.7(5) no C52 . C51 . H511 . 110.7(6) no C50 . C51 . H512 . 110.7(7) no C52 . C51 . H512 . 110.7(4) no H511 . C51 . H512 . 109.5(5) no C47 . C52 . C51 . 107.1(3) no C47 . C52 . C53 . 112.8(4) no C51 . C52 . C53 . 115.7(4) no C47 . C52 . C54 . 100.7(2) no C51 . C52 . C54 . 101.7(3) no C53 . C52 . C54 . 117.1(3) no C52 . C53 . H531 . 109.5(6) no C52 . C53 . H532 . 109.5(4) no H531 . C53 . H532 . 109.5(5) no C52 . C53 . H533 . 109.5(5) no H531 . C53 . H533 . 109.5(5) no H532 . C53 . H533 . 109.5(7) no C49 . C54 . C52 . 93.1(3) no C49 . C54 . C55 . 114.2(3) no C52 . C54 . C55 . 114.2(3) no C49 . C54 . C56 . 114.3(4) no C52 . C54 . C56 . 114.0(3) no C55 . C54 . C56 . 106.9(3) no C54 . C55 . H551 . 109.5(3) no C54 . C55 . H552 . 109.5(4) no H551 . C55 . H552 . 109.5(4) no C54 . C55 . H553 . 109.5(4) no H551 . C55 . H553 . 109.5(5) no H552 . C55 . H553 . 109.5(4) no C54 . C56 . H561 . 109.5(4) no C54 . C56 . H562 . 109.5(4) no H561 . C56 . H562 . 109.5(5) no C54 . C56 . H563 . 109.5(5) no H561 . C56 . H563 . 109.5(5) no H562 . C56 . H563 . 109.5(5) no data_const259 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H58 Ag2 F12 N6 O2 P2' _chemical_formula_weight 1304.72 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 24.641(7) _cell_length_b 12.669(2) _cell_length_c 8.390(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.59(3) _cell_angle_gamma 90.00 _cell_volume 2606.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method ? _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'STOE IPDS' _diffrn_measurement_method 'Image Plate' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6901 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 28.08 _reflns_number_total 4821 _reflns_number_observed 4773 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE_IPDS software' _computing_cell_refinement 'STOE_IPDS software' _computing_data_reduction 'STOE_IPDS software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SCHAKAL (Keller 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0486P)^2^+1.1634P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 4821 _refine_ls_number_parameters 376 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_obs 0.0253 _refine_ls_wR_factor_all 0.0702 _refine_ls_wR_factor_obs 0.0687 _refine_ls_goodness_of_fit_all 1.065 _refine_ls_goodness_of_fit_obs 1.048 _refine_ls_restrained_S_all 1.065 _refine_ls_restrained_S_obs 1.048 _refine_ls_shift/esd_max 0.020 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P P 0.35152(3) 0.17985(6) 0.96715(7) 0.0368(2) Uani 1 d . . F1 F 0.28743(8) 0.1719(3) 0.9450(3) 0.0632(6) Uani 1 d . . F2 F 0.41658(10) 0.1894(2) 0.9869(4) 0.0750(8) Uani 1 d . . F3 F 0.35688(12) 0.0538(2) 0.9600(3) 0.0595(6) Uani 1 d . . F4 F 0.35196(15) 0.1748(3) 1.1559(2) 0.0836(10) Uani 1 d . . F5 F 0.34823(11) 0.3062(2) 0.9708(3) 0.0560(6) Uani 1 d . . F6 F 0.35272(10) 0.1829(2) 0.7769(2) 0.0522(5) Uani 1 d . . Ag Ag 0.453663(5) 0.66217(2) 0.597764(15) 0.02815(7) Uani 1 d . . N1 N 0.47779(8) 0.8129(2) 0.7001(2) 0.0261(4) Uani 1 d . . C1 C 0.44246(10) 0.8919(2) 0.6674(3) 0.0294(5) Uani 1 d . . C2 C 0.45381(10) 0.9959(2) 0.7162(3) 0.0360(5) Uani 1 d . . H2 H 0.42815(10) 1.0501(2) 0.6941(3) 0.031(8) Uiso 1 calc R . C3 C 0.50380(11) 1.0156(2) 0.7974(4) 0.0382(6) Uani 1 d . . H3 H 0.51286(11) 1.0847(2) 0.8312(4) 0.052(11) Uiso 1 calc R . C4 C 0.54139(10) 0.9341(2) 0.8303(3) 0.0338(5) Uani 1 d . . H4 H 0.57577(10) 0.9476(2) 0.8852(3) 0.072(15) Uiso 1 calc R . C5 C 0.52699(9) 0.8330(2) 0.7803(3) 0.0273(4) Uani 1 d . . C6 C 0.56406(9) 0.7413(2) 0.8141(3) 0.0275(4) Uani 1 d . . C7 C 0.60355(10) 0.7417(3) 0.9470(3) 0.0350(5) Uani 1 d . . H7 H 0.60685(10) 0.7998(3) 1.0169(3) 0.039(9) Uiso 1 calc R . C8 C 0.63710(10) 0.6560(4) 0.9731(3) 0.0403(6) Uani 1 d . . H8 H 0.66457(10) 0.6561(4) 1.0591(3) 0.115(22) Uiso 1 calc R . C9 C 0.63061(10) 0.5690(3) 0.8729(3) 0.0351(5) Uani 1 d . . H9 H 0.65254(10) 0.5087(3) 0.8914(3) 0.067(14) Uiso 1 calc R . C10 C 0.59041(9) 0.5736(2) 0.7433(3) 0.0268(4) Uani 1 d . . N2 N 0.55839(6) 0.6585(2) 0.7155(2) 0.0258(3) Uani 1 d . . C11 C 0.58178(9) 0.4830(2) 0.6321(3) 0.0262(4) Uani 1 d . . N3 N 0.56876(7) 0.5027(2) 0.4747(2) 0.0251(4) Uani 1 d . . C12 C 0.56099(11) 0.4224(2) 0.3702(3) 0.0280(5) Uani 1 d . . C13 C 0.54911(12) 0.4491(3) 0.1954(3) 0.0373(5) Uani 1 d . . H13A H 0.5298(13) 0.3909(12) 0.1402(9) 0.129(28) Uiso 1 calc R . H13B H 0.58311(14) 0.4615(28) 0.1490(10) 0.088(19) Uiso 1 calc R . H13C H 0.5267(12) 0.5122(16) 0.1843(4) 0.045(10) Uiso 1 calc R . C14 C 0.56544(11) 0.3174(2) 0.4208(3) 0.0338(5) Uani 1 d . . H14 H 0.55956(11) 0.2619(2) 0.3467(3) 0.034(8) Uiso 1 calc R . C15 C 0.57854(11) 0.2964(2) 0.5809(4) 0.0371(5) Uani 1 d . . H15 H 0.58172(11) 0.2262(2) 0.6169(4) 0.051(11) Uiso 1 calc R . C16 C 0.58706(11) 0.3790(2) 0.6891(3) 0.0337(5) Uani 1 d . . H16 H 0.59619(11) 0.3655(2) 0.7986(3) 0.042(9) Uiso 1 calc R . O O 0.39604(7) 0.8589(2) 0.5854(2) 0.0358(4) Uani 1 d . . C17 C 0.34790(9) 0.9267(2) 0.5803(3) 0.0290(4) Uani 1 d . . H17 H 0.34443(9) 0.9567(2) 0.6877(3) 0.030(8) Uiso 1 calc R . C18 C 0.34600(10) 1.0161(2) 0.4546(3) 0.0339(5) Uani 1 d . . H18A H 0.34591(10) 1.0856(2) 0.5057(3) 0.037(9) Uiso 1 calc R . H18B H 0.37701(10) 1.0117(2) 0.3901(3) 0.044(10) Uiso 1 calc R . C19 C 0.29181(10) 0.9950(2) 0.3520(3) 0.0328(5) Uani 1 d . . H19 H 0.27591(10) 1.0576(2) 0.2945(3) 0.032(8) Uiso 1 calc R . C20 C 0.30142(12) 0.9006(3) 0.2440(3) 0.0368(5) Uani 1 d . . H20A H 0.33473(12) 0.9097(3) 0.1905(3) 0.053(11) Uiso 1 calc R . H20B H 0.27048(12) 0.8899(3) 0.1630(3) 0.043(10) Uiso 1 calc R . C21 C 0.30706(10) 0.8079(2) 0.3643(3) 0.0321(5) Uani 1 d . . H21A H 0.34345(10) 0.7762(2) 0.3681(3) 0.032(8) Uiso 1 calc R . H21B H 0.27971(10) 0.7534(2) 0.3350(3) 0.049(11) Uiso 1 calc R . C22 C 0.29772(9) 0.8584(2) 0.5273(3) 0.0284(4) Uani 1 d . . C23 C 0.28327(14) 0.7808(3) 0.6533(4) 0.0448(6) Uani 1 d . . H23A H 0.3115(7) 0.7274(15) 0.6688(28) 0.051(11) Uiso 1 calc R . H23B H 0.2487(7) 0.7476(19) 0.6187(18) 0.136(32) Uiso 1 calc R . H23C H 0.2804(13) 0.8178(5) 0.7534(11) 0.068(14) Uiso 1 calc R . C24 C 0.25598(10) 0.9473(2) 0.4744(3) 0.0311(4) Uani 1 d . . C25 C 0.20147(12) 0.9052(3) 0.3987(4) 0.0458(7) Uani 1 d . . H25A H 0.20786(12) 0.8509(19) 0.3212(30) 0.051(11) Uiso 1 calc R . H25B H 0.1807(6) 0.9624(6) 0.3455(35) 0.081(17) Uiso 1 calc R . H25C H 0.1811(6) 0.8755(24) 0.4814(7) 0.064(14) Uiso 1 calc R . C26 C 0.24381(12) 1.0219(3) 0.6104(4) 0.0424(7) Uani 1 d . . H26A H 0.2776(2) 1.0525(21) 0.6585(27) 0.082(18) Uiso 1 calc R . H26B H 0.2265(12) 0.9826(6) 0.6909(19) 0.083(18) Uiso 1 calc R . H26C H 0.2196(11) 1.0777(15) 0.5680(8) 0.067(14) Uiso 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 P 0.0427(3) 0.0342(5) 0.0313(3) 0.0051(2) -0.0082(2) -0.0044(3) F1 0.0440(9) 0.073(2) 0.0724(12) -0.0163(15) 0.0049(8) -0.0048(12) F2 0.0437(11) 0.067(2) 0.108(2) 0.0225(14) -0.0230(11) -0.0092(9) F3 0.078(2) 0.0322(12) 0.0639(12) 0.0115(9) -0.0149(11) -0.0021(10) F4 0.139(2) 0.077(2) 0.0307(7) 0.0065(11) -0.0098(10) -0.049(2) F5 0.082(2) 0.0349(12) 0.0479(10) -0.0031(9) -0.0122(10) 0.0003(10) F6 0.0763(12) 0.046(2) 0.0340(7) 0.0026(7) 0.0020(7) -0.0020(9) Ag 0.03070(9) 0.02411(10) 0.02891(9) -0.00459(7) -0.00078(5) -0.00249(7) N1 0.0239(9) 0.0249(10) 0.0287(8) -0.0051(7) -0.0014(7) 0.0004(7) C1 0.0247(11) 0.0253(13) 0.0374(12) -0.0089(10) -0.0010(9) 0.0002(8) C2 0.0313(12) 0.0270(14) 0.0485(14) -0.0084(11) -0.0020(10) 0.0019(9) C3 0.0334(13) 0.0298(14) 0.0509(14) -0.0125(11) 0.0008(10) -0.0035(10) C4 0.0270(10) 0.0332(14) 0.0403(12) -0.0120(10) -0.0009(8) -0.0010(9) C5 0.0229(9) 0.0312(13) 0.0274(9) -0.0065(8) 0.0010(7) -0.0012(8) C6 0.0262(10) 0.0311(12) 0.0251(9) -0.0024(8) 0.0015(8) 0.0009(8) C7 0.0319(11) 0.045(2) 0.0272(10) -0.0095(10) -0.0028(8) 0.0003(10) C8 0.0363(10) 0.054(2) 0.0280(8) -0.0021(15) -0.0082(7) 0.007(2) C9 0.0322(11) 0.043(2) 0.0288(10) 0.0024(10) -0.0054(9) 0.0087(10) C10 0.0252(10) 0.0315(13) 0.0237(9) 0.0031(8) 0.0016(7) 0.0024(8) N2 0.0236(7) 0.0291(9) 0.0243(6) -0.0028(10) 0.0006(5) 0.0015(10) C11 0.0250(10) 0.0271(12) 0.0262(9) 0.0043(8) 0.0010(7) 0.0055(8) N3 0.0236(8) 0.0264(10) 0.0247(8) 0.0012(7) -0.0001(6) 0.0037(7) C12 0.0273(11) 0.0270(13) 0.0297(11) -0.0021(9) 0.0021(8) 0.0047(9) C13 0.0435(14) 0.039(2) 0.0288(11) -0.0037(10) 0.0016(9) 0.0052(11) C14 0.0319(12) 0.0266(12) 0.0425(12) -0.0043(10) 0.0021(9) 0.0007(9) C15 0.0387(13) 0.0247(13) 0.0477(14) 0.0060(10) 0.0027(10) 0.0040(9) C16 0.0384(13) 0.0277(13) 0.0343(11) 0.0077(9) -0.0003(9) 0.0045(9) O 0.0281(8) 0.0256(9) 0.0507(10) -0.0109(8) -0.0107(7) 0.0040(7) C17 0.0237(10) 0.0238(12) 0.0385(11) -0.0035(8) -0.0015(8) 0.0017(8) C18 0.0291(11) 0.0243(12) 0.0480(13) 0.0013(10) 0.0022(9) -0.0029(8) C19 0.0321(11) 0.0246(12) 0.0409(11) 0.0026(10) -0.0014(9) 0.0030(9) C20 0.0407(13) 0.037(2) 0.0332(11) -0.0003(10) 0.0044(9) 0.0012(10) C21 0.0301(11) 0.0272(13) 0.0380(12) -0.0046(9) -0.0023(9) -0.0001(8) C22 0.0266(10) 0.0236(12) 0.0349(10) 0.0002(9) 0.0014(8) -0.0030(8) C23 0.057(2) 0.034(2) 0.0439(14) 0.0068(12) 0.0054(12) -0.0085(12) C24 0.0241(10) 0.0274(12) 0.0414(12) -0.0062(9) 0.0008(8) 0.0004(8) C25 0.0258(12) 0.050(2) 0.060(2) -0.0145(15) -0.0017(11) -0.0030(11) C26 0.0331(13) 0.040(2) 0.055(2) -0.0158(13) 0.0073(11) 0.0031(11) _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 P F1 1.575(2) . ? P F4 1.584(2) . ? P F6 1.600(2) . ? P F2 1.600(3) . ? P F3 1.603(3) . ? P F5 1.604(2) . ? Ag N1 2.153(2) . ? Ag N3 2.165(2) 2_656 ? Ag N2 2.616(2) 2_656 ? Ag Ag 2.9387(10) 2_656 ? N1 C1 1.337(3) . ? N1 C5 1.352(3) . ? C1 O 1.343(3) . ? C1 C2 1.399(4) . ? C2 C3 1.371(4) . ? C3 C4 1.397(4) . ? C4 C5 1.383(4) . ? C5 C6 1.487(3) . ? C6 N2 1.335(4) . ? C6 C7 1.407(3) . ? C7 C8 1.369(5) . ? C8 C9 1.386(5) . ? C9 C10 1.399(3) . ? C10 N2 1.341(3) . ? C10 C11 1.481(3) . ? N2 Ag 2.616(2) 2_656 ? C11 N3 1.351(3) . ? C11 C16 1.404(4) . ? N3 C12 1.345(3) . ? N3 Ag 2.165(2) 2_656 ? C12 C14 1.398(4) . ? C12 C13 1.506(4) . ? C14 C15 1.376(4) . ? C15 C16 1.388(4) . ? O C17 1.462(3) . ? C17 C22 1.539(3) . ? C17 C18 1.545(4) . ? C18 C19 1.540(4) . ? C19 C20 1.533(4) . ? C19 C24 1.541(4) . ? C20 C21 1.546(4) . ? C21 C22 1.547(3) . ? C22 C23 1.511(4) . ? C22 C24 1.561(4) . ? C24 C25 1.525(4) . ? C24 C26 1.534(4) . ? 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 F1 P F4 91.4(2) . . ? F1 P F6 89.98(13) . . ? F4 P F6 178.3(2) . . ? F1 P F2 178.9(2) . . ? F4 P F2 89.5(2) . . ? F6 P F2 89.18(15) . . ? F1 P F3 91.0(2) . . ? F4 P F3 90.3(2) . . ? F6 P F3 88.71(13) . . ? F2 P F3 89.7(2) . . ? F1 P F5 90.8(2) . . ? F4 P F5 90.9(2) . . ? F6 P F5 90.04(12) . . ? F2 P F5 88.5(2) . . ? F3 P F5 177.8(2) . . ? N1 Ag N3 172.75(7) . 2_656 ? N1 Ag N2 114.60(8) . 2_656 ? N3 Ag N2 72.57(8) 2_656 2_656 ? N1 Ag Ag 91.33(5) . 2_656 ? N3 Ag Ag 91.95(5) 2_656 2_656 ? N2 Ag Ag 57.15(4) 2_656 2_656 ? C1 N1 C5 119.7(2) . . ? C1 N1 Ag 115.7(2) . . ? C5 N1 Ag 124.4(2) . . ? N1 C1 O 112.1(2) . . ? N1 C1 C2 122.5(2) . . ? O C1 C2 125.4(2) . . ? C3 C2 C1 117.5(3) . . ? C2 C3 C4 120.6(3) . . ? C5 C4 C3 118.6(2) . . ? N1 C5 C4 121.1(2) . . ? N1 C5 C6 116.9(2) . . ? C4 C5 C6 122.0(2) . . ? N2 C6 C7 121.1(2) . . ? N2 C6 C5 118.0(2) . . ? C7 C6 C5 120.9(2) . . ? C8 C7 C6 119.0(3) . . ? C7 C8 C9 120.1(2) . . ? C8 C9 C10 118.0(3) . . ? N2 C10 C9 122.0(2) . . ? N2 C10 C11 117.8(2) . . ? C9 C10 C11 120.3(2) . . ? C6 N2 C10 119.9(2) . . ? C6 N2 Ag 127.1(2) . 2_656 ? C10 N2 Ag 101.32(13) . 2_656 ? N3 C11 C16 120.8(2) . . ? N3 C11 C10 118.5(2) . . ? C16 C11 C10 120.7(2) . . ? C12 N3 C11 120.2(2) . . ? C12 N3 Ag 120.4(2) . 2_656 ? C11 N3 Ag 118.5(2) . 2_656 ? N3 C12 C14 121.3(2) . . ? N3 C12 C13 117.8(2) . . ? C14 C12 C13 120.8(2) . . ? C15 C14 C12 119.0(3) . . ? C14 C15 C16 119.9(3) . . ? C15 C16 C11 118.8(2) . . ? C1 O C17 118.7(2) . . ? O C17 C22 107.8(2) . . ? O C17 C18 114.9(2) . . ? C22 C17 C18 104.2(2) . . ? C19 C18 C17 102.8(2) . . ? C20 C19 C18 106.9(2) . . ? C20 C19 C24 102.7(2) . . ? C18 C19 C24 102.6(2) . . ? C19 C20 C21 102.4(2) . . ? C20 C21 C22 104.6(2) . . ? C23 C22 C17 113.6(2) . . ? C23 C22 C21 114.5(2) . . ? C17 C22 C21 107.6(2) . . ? C23 C22 C24 118.3(2) . . ? C17 C22 C24 99.5(2) . . ? C21 C22 C24 101.4(2) . . ? C25 C24 C26 107.3(2) . . ? C25 C24 C19 113.5(2) . . ? C26 C24 C19 114.9(2) . . ? C25 C24 C22 113.3(2) . . ? C26 C24 C22 113.8(2) . . ? C19 C24 C22 93.9(2) . . ? _refine_diff_density_max 0.513 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.048