Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' loop_ _publ_author_name 'Miyazaki, Hirofumi' 'Ooyama, Yousuke' 'Watanabe, Shigeru' 'Yoshida, Katsuhira' _publ_contact_author_name 'Prof Katsuhira Yoshida' _publ_contact_author_address ; Department of Material Science Kochi University Akebono-cho Kochi 780 8520 JAPAN ; _publ_contact_author_email 'KYOSHIDA@CC.KOCHI-U.AC.JP' #------------------------------------------------------------------------------ _publ_requested_journal 'Journal of the Chemical Society; Perkin Transactions 2' _publ_section_title ; Heterocyclicquinol-type fluorophores. Part 1. Synthesis of new benzofurano[3, 2-b]-naphthoquinol delivatives and their photophysical properties in solution and in the crystalline state ; data_ 2c _database_code_CSD 172460 #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_formula_sum 'C30 H31 N O3 ' _chemical_formula_weight 453.58 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/n ' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _cell_length_a 11.083(7) _cell_length_b 15.859(8) _cell_length_c 14.244(8) _cell_angle_alpha 90 _cell_angle_beta 97.56(5) _cell_angle_gamma 90 _cell_volume 2481(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.214 _diffrn_radiation_type 'Mo K¥a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.3 _cell_measurement_theta_max 14.9 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_F_000 968.00 _exptl_absorpt_coefficient_mu 0.077 _exptl_crystal_description 'prismatic' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.400 _exptl_crystal_colour 'orange' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method ¥w-2¥q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.688 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_radiation_monochromator graphite _diffrn_reflns_number 4534 _reflns_number_total 4353 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 0 #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.085 _refine_ls_number_reflns 2616 _refine_ls_number_parameters 420 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[¥s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0040 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.18 _refine_diff_density_max 0.31 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 1.1306(2) 0.1782(2) 0.4307(2) 0.0579(8) Uani 1.00 d . . . O(2) O 0.7723(2) -0.0258(2) 0.4915(2) 0.0589(8) Uani 1.00 d . . . O(3) O 0.8999(2) -0.0529(1) 0.3334(2) 0.0503(7) Uani 1.00 d . . . N(1) N 1.1101(4) -0.1293(2) 0.0701(3) 0.091(1) Uani 1.00 d . . . C(1) C 0.8380(3) 0.0301(2) 0.4644(2) 0.0466(9) Uani 1.00 d . . . C(2) C 0.8537(3) 0.1136(2) 0.5118(2) 0.0470(10) Uani 1.00 d . . . C(3) C 0.7887(4) 0.1302(3) 0.5876(3) 0.061(1) Uani 1.00 d . . . C(4) C 0.8009(4) 0.2062(3) 0.6336(3) 0.074(1) Uani 1.00 d . . . C(5) C 0.8779(5) 0.2674(3) 0.6049(3) 0.077(2) Uani 1.00 d . . . C(6) C 0.9422(4) 0.2510(3) 0.5311(3) 0.066(1) Uani 1.00 d . . . C(7) C 0.9310(3) 0.1752(2) 0.4831(2) 0.0487(10) Uani 1.00 d . . . C(8) C 1.0049(3) 0.1633(2) 0.4003(2) 0.0469(10) Uani 1.00 d . . . C(9) C 0.9867(3) 0.0762(2) 0.3582(2) 0.0447(9) Uani 1.00 d . . . C(10) C 1.0377(3) 0.0376(2) 0.2824(2) 0.0477(10) Uani 1.00 d . . . C(11) C 1.1250(4) 0.0586(2) 0.2240(3) 0.063(1) Uani 1.00 d . . . C(12) C 1.1491(4) 0.0025(3) 0.1562(3) 0.072(1) Uani 1.00 d . . . C(13) C 1.0859(4) -0.0760(2) 0.1407(3) 0.065(1) Uani 1.00 d . . . C(14) C 1.0000(4) -0.0975(2) 0.1999(3) 0.055(1) Uani 1.00 d . . . C(15) C 0.9803(3) -0.0404(2) 0.2684(2) 0.0467(10) Uani 1.00 d . . . C(16) C 0.9058(3) 0.0202(2) 0.3868(2) 0.0453(9) Uani 1.00 d . . . C(17) C 0.9622(3) 0.2278(2) 0.3229(2) 0.049(1) Uani 1.00 d . . . C(18) C 1.0415(4) 0.2864(2) 0.2934(3) 0.062(1) Uani 1.00 d . . . C(19) C 0.9984(5) 0.3442(3) 0.2231(4) 0.083(2) Uani 1.00 d . . . C(20) C 0.8800(5) 0.3434(3) 0.1830(3) 0.081(2) Uani 1.00 d . . . C(21) C 0.8016(5) 0.2848(3) 0.2112(3) 0.077(2) Uani 1.00 d . . . C(22) C 0.8419(4) 0.2280(3) 0.2810(3) 0.064(1) Uani 1.00 d . . . C(23) C 1.2221(6) -0.1151(4) 0.0173(4) 0.100(2) Uani 1.00 d . . . C(24) C 1.1809(8) -0.0671(5) -0.0644(5) 0.128(3) Uani 1.00 d . . . C(25) C 1.3020(9) -0.0504(7) -0.1165(7) 0.156(4) Uani 1.00 d . . . C(26) C 1.3504(8) 0.0272(6) -0.0833(7) 0.191(5) Uani 1.00 d . . . C(27) C 1.0332(5) -0.2020(3) 0.0429(4) 0.082(2) Uani 1.00 d . . . C(28) C 1.0713(4) -0.2791(3) 0.1030(4) 0.079(2) Uani 1.00 d . . . C(29) C 0.9868(5) -0.3525(4) 0.0780(5) 0.102(2) Uani 1.00 d . . . C(30) C 1.0215(7) -0.4292(4) 0.1365(6) 0.127(3) Uani 1.00 d . . . H(1) H 1.158(5) 0.133(4) 0.461(4) 0.14(2) Uiso 1.00 calc . . . H(2) H 0.730(3) 0.085(2) 0.607(2) 0.046(9) Uiso 1.00 calc . . . H(3) H 0.759(3) 0.215(2) 0.686(3) 0.07(1) Uiso 1.00 calc . . . H(4) H 0.893(4) 0.321(3) 0.640(3) 0.08(1) Uiso 1.00 calc . . . H(5) H 0.996(4) 0.292(3) 0.508(3) 0.09(1) Uiso 1.00 calc . . . H(6) H 1.168(3) 0.115(2) 0.234(2) 0.06(1) Uiso 1.00 calc . . . H(7) H 1.196(4) 0.016(3) 0.111(3) 0.11(2) Uiso 1.00 calc . . . H(8) H 0.951(3) -0.152(2) 0.195(2) 0.042(8) Uiso 1.00 calc . . . H(9) H 1.120(3) 0.286(2) 0.327(2) 0.06(1) Uiso 1.00 calc . . . H(10) H 1.062(5) 0.387(3) 0.207(4) 0.13(2) Uiso 1.00 calc . . . H(11) H 0.854(4) 0.386(3) 0.135(3) 0.09(1) Uiso 1.00 calc . . . H(12) H 0.714(4) 0.281(3) 0.183(3) 0.09(1) Uiso 1.00 calc . . . H(13) H 0.794(4) 0.188(2) 0.299(3) 0.07(1) Uiso 1.00 calc . . . H(14) H 1.260(5) -0.171(4) -0.012(4) 0.16(2) Uiso 1.00 calc . . . H(15) H 1.301(5) -0.087(4) 0.060(4) 0.14(2) Uiso 1.00 calc . . . H(16) H 1.110(6) -0.105(4) -0.116(4) 0.15(2) Uiso 1.00 calc . . . H(17) H 1.147(4) -0.013(3) -0.046(3) 0.10(2) Uiso 1.00 calc . . . H(18) H 1.386(6) -0.078(4) -0.129(5) 0.16(2) Uiso 1.00 calc . . . H(19) H 1.342(5) -0.027(4) -0.176(4) 0.12(2) Uiso 1.00 calc . . . H(20) H 1.3241 0.0414 -0.0161 0.2219 Uiso 1.00 calc . . . H(21) H 1.4332 0.0353 -0.0737 0.2219 Uiso 1.00 calc . . . H(22) H 1.3132 0.0782 -0.1178 0.2219 Uiso 1.00 calc . . . H(23) H 0.938(4) -0.189(2) 0.043(3) 0.08(1) Uiso 1.00 calc . . . H(24) H 1.044(4) -0.219(3) -0.016(3) 0.10(2) Uiso 1.00 calc . . . H(25) H 1.075(4) -0.267(3) 0.176(4) 0.12(2) Uiso 1.00 calc . . . H(26) H 1.159(5) -0.298(3) 0.089(4) 0.15(2) Uiso 1.00 calc . . . H(27) H 0.905(6) -0.324(4) 0.099(5) 0.19(2) Uiso 1.00 calc . . . H(28) H 0.980(7) -0.364(5) -0.008(6) 0.21(2) Uiso 1.00 calc . . . H(29) H 1.121(8) -0.426(5) 0.170(7) 0.24(2) Uiso 1.00 calc . . . H(30) H 0.963(8) -0.465(6) 0.130(7) 0.24(1) Uiso 1.00 calc . . . H(31) H 1.019(8) -0.406(5) 0.217(6) 0.23(2) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(1) 0.046(1) 0.049(1) 0.077(2) -0.009(1) 0.001(1) 0.005(1) O(2) 0.055(1) 0.057(2) 0.066(2) -0.009(1) 0.015(1) 0.007(1) O(3) 0.050(1) 0.043(1) 0.060(1) -0.006(1) 0.012(1) -0.001(1) N(1) 0.118(3) 0.072(2) 0.097(3) -0.019(2) 0.065(3) -0.024(2) C(1) 0.039(2) 0.049(2) 0.051(2) -0.001(2) 0.000(2) 0.009(2) C(2) 0.040(2) 0.052(2) 0.049(2) 0.002(2) 0.003(2) 0.004(2) C(3) 0.064(3) 0.065(3) 0.053(2) -0.003(2) 0.010(2) 0.000(2) C(4) 0.085(3) 0.085(3) 0.055(2) -0.005(3) 0.025(2) -0.013(2) C(5) 0.103(4) 0.065(3) 0.066(3) -0.010(3) 0.019(3) -0.017(2) C(6) 0.082(3) 0.059(3) 0.060(2) -0.011(2) 0.019(2) -0.007(2) C(7) 0.053(2) 0.047(2) 0.046(2) -0.001(2) 0.005(2) 0.001(2) C(8) 0.046(2) 0.041(2) 0.054(2) -0.005(1) 0.007(2) -0.001(2) C(9) 0.043(2) 0.042(2) 0.049(2) 0.000(1) 0.004(2) 0.005(2) C(10) 0.048(2) 0.043(2) 0.054(2) 0.000(2) 0.009(2) 0.002(2) C(11) 0.067(3) 0.048(2) 0.079(3) -0.009(2) 0.029(2) -0.002(2) C(12) 0.079(3) 0.063(3) 0.080(3) -0.008(2) 0.039(2) -0.003(2) C(13) 0.079(3) 0.052(2) 0.069(3) 0.000(2) 0.025(2) -0.003(2) C(14) 0.061(2) 0.045(2) 0.060(2) -0.004(2) 0.013(2) 0.000(2) C(15) 0.046(2) 0.045(2) 0.051(2) 0.002(2) 0.010(2) 0.004(2) C(16) 0.044(2) 0.041(2) 0.052(2) -0.003(1) 0.009(2) -0.001(2) C(17) 0.061(2) 0.039(2) 0.049(2) 0.006(2) 0.011(2) 0.000(2) C(18) 0.068(3) 0.056(2) 0.066(2) 0.005(2) 0.023(2) 0.014(2) C(19) 0.102(4) 0.069(3) 0.086(3) 0.018(3) 0.040(3) 0.027(3) C(20) 0.106(4) 0.071(3) 0.070(3) 0.034(3) 0.024(3) 0.023(2) C(21) 0.079(3) 0.073(3) 0.075(3) 0.025(3) 0.001(3) 0.007(2) C(22) 0.060(3) 0.056(2) 0.075(3) 0.005(2) 0.002(2) 0.009(2) C(23) 0.114(5) 0.083(4) 0.098(4) 0.028(3) -0.008(4) -0.009(3) C(24) 0.152(6) 0.110(5) 0.112(5) 0.028(5) -0.019(5) 0.001(4) C(25) 0.164(8) 0.165(8) 0.159(7) -0.054(6) 0.091(6) 0.000(6) C(26) 0.186(9) 0.186(9) 0.204(10) -0.054(7) 0.038(7) 0.048(8) C(27) 0.102(4) 0.073(3) 0.074(3) -0.010(3) 0.030(3) -0.021(3) C(28) 0.067(3) 0.066(3) 0.105(4) -0.002(2) 0.020(3) -0.018(3) C(29) 0.094(4) 0.081(4) 0.128(5) -0.017(3) 0.007(4) -0.008(4) C(30) 0.139(6) 0.077(4) 0.161(6) -0.018(4) 0.005(5) 0.016(4) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(8) 1.423(4) 1_555 1_555 yes O(2) C(1) 1.240(4) 1_555 1_555 yes O(3) C(15) 1.381(4) 1_555 1_555 yes O(3) C(16) 1.384(4) 1_555 1_555 yes N(1) C(13) 1.366(5) 1_555 1_555 yes N(1) C(23) 1.551(7) 1_555 1_555 yes N(1) C(27) 1.456(6) 1_555 1_555 yes C(1) C(2) 1.486(5) 1_555 1_555 yes C(1) C(16) 1.425(4) 1_555 1_555 yes C(2) C(3) 1.400(5) 1_555 1_555 yes C(2) C(7) 1.395(4) 1_555 1_555 yes C(3) C(4) 1.371(6) 1_555 1_555 yes C(4) C(5) 1.389(6) 1_555 1_555 yes C(5) C(6) 1.370(6) 1_555 1_555 yes C(6) C(7) 1.381(5) 1_555 1_555 yes C(7) C(8) 1.533(4) 1_555 1_555 yes C(8) C(9) 1.508(4) 1_555 1_555 yes C(8) C(17) 1.533(4) 1_555 1_555 yes C(9) C(10) 1.423(4) 1_555 1_555 yes C(9) C(16) 1.362(4) 1_555 1_555 yes C(10) C(11) 1.396(5) 1_555 1_555 yes C(10) C(15) 1.393(4) 1_555 1_555 yes C(11) C(12) 1.365(6) 1_555 1_555 yes C(12) C(13) 1.431(5) 1_555 1_555 yes C(13) C(14) 1.395(5) 1_555 1_555 yes C(14) C(15) 1.370(5) 1_555 1_555 yes C(17) C(18) 1.382(5) 1_555 1_555 yes C(17) C(22) 1.387(5) 1_555 1_555 yes C(18) C(19) 1.396(6) 1_555 1_555 yes C(19) C(20) 1.360(7) 1_555 1_555 yes C(20) C(21) 1.368(7) 1_555 1_555 yes C(21) C(22) 1.372(6) 1_555 1_555 yes C(23) C(24) 1.414(8) 1_555 1_555 yes C(24) C(25) 1.64(1) 1_555 1_555 yes C(25) C(26) 1.40(1) 1_555 1_555 yes C(27) C(28) 1.521(7) 1_555 1_555 yes C(28) C(29) 1.507(7) 1_555 1_555 yes C(29) C(30) 1.496(9) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(8) O(1) H(1) 105(3) 1_555 1_555 1_555 no C(15) O(3) C(16) 105.1(2) 1_555 1_555 1_555 yes C(13) N(1) C(23) 121.0(4) 1_555 1_555 1_555 yes C(13) N(1) C(27) 121.4(4) 1_555 1_555 1_555 yes C(23) N(1) C(27) 117.6(4) 1_555 1_555 1_555 yes O(2) C(1) C(2) 122.4(3) 1_555 1_555 1_555 yes O(2) C(1) C(16) 123.6(3) 1_555 1_555 1_555 yes C(2) C(1) C(16) 114.1(3) 1_555 1_555 1_555 yes C(1) C(2) C(3) 118.4(3) 1_555 1_555 1_555 yes C(1) C(2) C(7) 122.0(3) 1_555 1_555 1_555 yes C(3) C(2) C(7) 119.6(3) 1_555 1_555 1_555 yes C(2) C(3) C(4) 120.3(4) 1_555 1_555 1_555 yes C(2) C(3) H(2) 118(1) 1_555 1_555 1_555 no C(4) C(3) H(2) 120(1) 1_555 1_555 1_555 no C(3) C(4) C(5) 120.0(4) 1_555 1_555 1_555 yes C(3) C(4) H(3) 118(2) 1_555 1_555 1_555 no C(5) C(4) H(3) 121(2) 1_555 1_555 1_555 no C(4) C(5) C(6) 119.7(4) 1_555 1_555 1_555 yes C(4) C(5) H(4) 121(2) 1_555 1_555 1_555 no C(6) C(5) H(4) 118(2) 1_555 1_555 1_555 no C(5) C(6) C(7) 121.6(4) 1_555 1_555 1_555 yes C(5) C(6) H(5) 122(2) 1_555 1_555 1_555 no C(7) C(6) H(5) 116(2) 1_555 1_555 1_555 no C(2) C(7) C(6) 118.8(3) 1_555 1_555 1_555 yes C(2) C(7) C(8) 123.4(3) 1_555 1_555 1_555 yes C(6) C(7) C(8) 117.8(3) 1_555 1_555 1_555 yes O(1) C(8) C(7) 110.3(3) 1_555 1_555 1_555 yes O(1) C(8) C(9) 110.3(3) 1_555 1_555 1_555 yes O(1) C(8) C(17) 107.8(3) 1_555 1_555 1_555 yes C(7) C(8) C(9) 111.2(3) 1_555 1_555 1_555 yes C(7) C(8) C(17) 109.0(3) 1_555 1_555 1_555 yes C(9) C(8) C(17) 108.2(3) 1_555 1_555 1_555 yes C(8) C(9) C(10) 130.6(3) 1_555 1_555 1_555 yes C(8) C(9) C(16) 122.5(3) 1_555 1_555 1_555 yes C(10) C(9) C(16) 106.8(3) 1_555 1_555 1_555 yes C(9) C(10) C(11) 136.5(3) 1_555 1_555 1_555 yes C(9) C(10) C(15) 105.7(3) 1_555 1_555 1_555 yes C(11) C(10) C(15) 117.8(3) 1_555 1_555 1_555 yes C(10) C(11) C(12) 118.7(4) 1_555 1_555 1_555 yes C(10) C(11) H(6) 118(1) 1_555 1_555 1_555 no C(12) C(11) H(6) 122(1) 1_555 1_555 1_555 no C(11) C(12) C(13) 122.7(4) 1_555 1_555 1_555 yes C(11) C(12) H(7) 121(3) 1_555 1_555 1_555 no C(13) C(12) H(7) 114(3) 1_555 1_555 1_555 no N(1) C(13) C(12) 120.8(4) 1_555 1_555 1_555 yes N(1) C(13) C(14) 120.6(4) 1_555 1_555 1_555 yes C(12) C(13) C(14) 118.6(4) 1_555 1_555 1_555 yes C(13) C(14) C(15) 117.1(3) 1_555 1_555 1_555 yes C(13) C(14) H(8) 124(1) 1_555 1_555 1_555 no C(15) C(14) H(8) 118(1) 1_555 1_555 1_555 no O(3) C(15) C(10) 110.8(3) 1_555 1_555 1_555 yes O(3) C(15) C(14) 124.0(3) 1_555 1_555 1_555 yes C(10) C(15) C(14) 125.2(3) 1_555 1_555 1_555 yes O(3) C(16) C(1) 121.8(3) 1_555 1_555 1_555 yes O(3) C(16) C(9) 111.6(3) 1_555 1_555 1_555 yes C(1) C(16) C(9) 126.5(3) 1_555 1_555 1_555 yes C(8) C(17) C(18) 121.2(3) 1_555 1_555 1_555 yes C(8) C(17) C(22) 120.0(3) 1_555 1_555 1_555 yes C(18) C(17) C(22) 118.7(4) 1_555 1_555 1_555 yes C(17) C(18) C(19) 119.3(4) 1_555 1_555 1_555 yes C(17) C(18) H(9) 115(2) 1_555 1_555 1_555 no C(19) C(18) H(9) 125(2) 1_555 1_555 1_555 no C(18) C(19) C(20) 121.0(5) 1_555 1_555 1_555 yes C(18) C(19) H(10) 114(3) 1_555 1_555 1_555 no C(20) C(19) H(10) 124(3) 1_555 1_555 1_555 no C(19) C(20) C(21) 119.8(5) 1_555 1_555 1_555 yes C(19) C(20) H(11) 118(2) 1_555 1_555 1_555 no C(21) C(20) H(11) 122(2) 1_555 1_555 1_555 no C(20) C(21) C(22) 120.0(5) 1_555 1_555 1_555 yes C(20) C(21) H(12) 122(2) 1_555 1_555 1_555 no C(22) C(21) H(12) 117(2) 1_555 1_555 1_555 no C(17) C(22) C(21) 121.1(4) 1_555 1_555 1_555 yes C(17) C(22) H(13) 116(2) 1_555 1_555 1_555 no C(21) C(22) H(13) 121(2) 1_555 1_555 1_555 no N(1) C(23) C(24) 106.5(5) 1_555 1_555 1_555 yes N(1) C(23) H(14) 116(3) 1_555 1_555 1_555 no N(1) C(23) H(15) 115(2) 1_555 1_555 1_555 no C(24) C(23) H(14) 102(3) 1_555 1_555 1_555 no C(24) C(23) H(15) 112(2) 1_555 1_555 1_555 no H(14) C(23) H(15) 103(4) 1_555 1_555 1_555 no C(23) C(24) C(25) 105.3(7) 1_555 1_555 1_555 yes C(23) C(24) H(16) 110(2) 1_555 1_555 1_555 no C(23) C(24) H(17) 110(2) 1_555 1_555 1_555 no C(25) C(24) H(16) 108(2) 1_555 1_555 1_555 no C(25) C(24) H(17) 109(2) 1_555 1_555 1_555 no H(16) C(24) H(17) 111(4) 1_555 1_555 1_555 no C(24) C(25) C(26) 106.8(8) 1_555 1_555 1_555 yes C(24) C(25) H(18) 142(4) 1_555 1_555 1_555 no C(24) C(25) H(19) 149(3) 1_555 1_555 1_555 no C(26) C(25) H(18) 96(3) 1_555 1_555 1_555 no C(26) C(25) H(19) 77(3) 1_555 1_555 1_555 no H(18) C(25) H(19) 63(3) 1_555 1_555 1_555 no C(25) C(26) H(20) 110.7(8) 1_555 1_555 1_555 no C(25) C(26) H(21) 120(1) 1_555 1_555 1_555 no C(25) C(26) H(22) 115(1) 1_555 1_555 1_555 no H(20) C(26) H(21) 102.9(10) 1_555 1_555 1_555 no H(20) C(26) H(22) 97.2(9) 1_555 1_555 1_555 no H(21) C(26) H(22) 107.2(8) 1_555 1_555 1_555 no N(1) C(27) C(28) 112.2(4) 1_555 1_555 1_555 yes N(1) C(27) H(23) 113(2) 1_555 1_555 1_555 no N(1) C(27) H(24) 110(3) 1_555 1_555 1_555 no C(28) C(27) H(23) 110(2) 1_555 1_555 1_555 no C(28) C(27) H(24) 102(3) 1_555 1_555 1_555 no H(23) C(27) H(24) 107(3) 1_555 1_555 1_555 no C(27) C(28) C(29) 111.7(4) 1_555 1_555 1_555 yes C(27) C(28) H(25) 112(2) 1_555 1_555 1_555 no C(27) C(28) H(26) 108(3) 1_555 1_555 1_555 no C(29) C(28) H(25) 108(2) 1_555 1_555 1_555 no C(29) C(28) H(26) 106(2) 1_555 1_555 1_555 no H(25) C(28) H(26) 108(3) 1_555 1_555 1_555 no C(28) C(29) C(30) 113.0(5) 1_555 1_555 1_555 yes C(28) C(29) H(27) 97(3) 1_555 1_555 1_555 no C(28) C(29) H(28) 107(3) 1_555 1_555 1_555 no C(30) C(29) H(27) 110(3) 1_555 1_555 1_555 no C(30) C(29) H(28) 114(3) 1_555 1_555 1_555 no H(27) C(29) H(28) 112(5) 1_555 1_555 1_555 no C(29) C(30) H(29) 110(4) 1_555 1_555 1_555 no C(29) C(30) H(30) 110(6) 1_555 1_555 1_555 no C(29) C(30) H(31) 104(3) 1_555 1_555 1_555 no H(29) C(30) H(30) 138(7) 1_555 1_555 1_555 no H(29) C(30) H(31) 74(5) 1_555 1_555 1_555 no H(30) C(30) H(31) 100(7) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ #===============================================END data_3c _database_code_CSD 172461 #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_formula_sum 'C30 H31 N O3 ' _chemical_formula_weight 453.58 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _cell_length_a 11.738(2) _cell_length_b 12.244(2) _cell_length_c 10.879(2) _cell_angle_alpha 90.69(2) _cell_angle_beta 116.39(1) _cell_angle_gamma 64.73(1) _cell_volume 1235.8(5) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.219 _diffrn_radiation_type 'Mo K¥a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.6 _cell_measurement_theta_max 14.8 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_F_000 484.00 _exptl_absorpt_coefficient_mu 0.078 _exptl_crystal_description 'prismatic' _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.550 _exptl_crystal_size_min 0.10 _exptl_crystal_colour 'orange' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method ¥w-2¥q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.975 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_radiation_monochromator graphite _diffrn_reflns_number 4577 _reflns_number_total 4345 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0494 _refine_ls_wR_factor_gt 0.0494 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.373 _refine_ls_number_reflns 2573 _refine_ls_number_parameters 432 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[¥s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0520 _refine_ls_shift/su_mean 0.0020 _refine_diff_density_min -0.14 _refine_diff_density_max 0.19 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.8619(2) 0.4125(2) 0.1698(2) 0.0521(5) Uani 1.00 d . . . O(2) O 0.3820(2) 0.4002(2) -0.1716(2) 0.0553(5) Uani 1.00 d . . . O(3) O 0.8357(2) 0.1881(2) 0.2095(2) 0.0464(5) Uani 1.00 d . . . N(1) N 0.7466(2) -0.1197(2) 0.3754(2) 0.0527(7) Uani 1.00 d . . . C(1) C 0.8090(2) 0.3555(2) 0.0577(3) 0.0434(7) Uani 1.00 d . . . C(2) C 0.6903(2) 0.4532(2) -0.0788(3) 0.0453(7) Uani 1.00 d . . . C(3) C 0.7232(3) 0.5333(3) -0.1294(3) 0.0581(9) Uani 1.00 d . . . C(4) C 0.6232(4) 0.6204(3) -0.2536(4) 0.069(1) Uani 1.00 d . . . C(5) C 0.4875(4) 0.6298(3) -0.3308(4) 0.073(1) Uani 1.00 d . . . C(6) C 0.4523(3) 0.5530(3) -0.2821(3) 0.0603(9) Uani 1.00 d . . . C(7) C 0.5523(2) 0.4639(2) -0.1563(3) 0.0463(7) Uani 1.00 d . . . C(8) C 0.5065(2) 0.3856(2) -0.1081(2) 0.0436(7) Uani 1.00 d . . . C(9) C 0.6163(2) 0.2908(2) 0.0187(2) 0.0414(7) Uani 1.00 d . . . C(10) C 0.6157(2) 0.1948(2) 0.0929(2) 0.0416(7) Uani 1.00 d . . . C(11) C 0.5197(2) 0.1498(2) 0.0751(3) 0.0452(7) Uani 1.00 d . . . C(12) C 0.5645(3) 0.0476(2) 0.1690(3) 0.0461(7) Uani 1.00 d . . . C(13) C 0.7060(2) -0.0152(2) 0.2864(3) 0.0453(7) Uani 1.00 d . . . C(14) C 0.8011(3) 0.0325(2) 0.3067(3) 0.0462(7) Uani 1.00 d . . . C(15) C 0.7525(2) 0.1336(2) 0.2086(2) 0.0421(7) Uani 1.00 d . . . C(16) C 0.7484(2) 0.2824(2) 0.0917(2) 0.0414(7) Uani 1.00 d . . . C(17) C 0.9364(2) 0.2696(2) 0.0365(3) 0.0426(7) Uani 1.00 d . . . C(18) C 0.9225(3) 0.1884(3) -0.0510(3) 0.0611(9) Uani 1.00 d . . . C(19) C 1.0339(3) 0.1131(3) -0.0753(4) 0.067(1) Uani 1.00 d . . . C(20) C 1.1614(3) 0.1177(3) -0.0121(3) 0.0609(9) Uani 1.00 d . . . C(21) C 1.1764(3) 0.1979(3) 0.0754(4) 0.069(1) Uani 1.00 d . . . C(22) C 1.0650(3) 0.2730(3) 0.1006(3) 0.0580(9) Uani 1.00 d . . . C(23) C 0.6510(3) -0.1746(3) 0.3454(3) 0.0545(9) Uani 1.00 d . . . C(24) C 0.5379(3) -0.1137(3) 0.3913(3) 0.0564(9) Uani 1.00 d . . . C(25) C 0.4287(4) -0.1618(4) 0.3415(4) 0.067(1) Uani 1.00 d . . . C(26) C 0.3070(4) -0.0920(4) 0.3744(5) 0.076(1) Uani 1.00 d . . . C(27) C 0.8925(3) -0.1861(3) 0.4949(3) 0.0609(9) Uani 1.00 d . . . C(28) C 1.0074(4) -0.2667(4) 0.4567(4) 0.082(1) Uani 1.00 d . . . C(29) C 0.9779(5) -0.3596(4) 0.3771(5) 0.112(2) Uani 1.00 d . . . C(30) C 1.0998(6) -0.4427(6) 0.3474(7) 0.127(2) Uani 1.00 d . . . H(1) H 0.784(4) 0.473(3) 0.172(3) 0.11(1) Uiso 1.00 calc . . . H(2) H 0.815(3) 0.529(2) -0.074(3) 0.069(8) Uiso 1.00 calc . . . H(3) H 0.648(3) 0.676(3) -0.285(3) 0.086(10) Uiso 1.00 calc . . . H(4) H 0.412(3) 0.692(3) -0.424(3) 0.094(10) Uiso 1.00 calc . . . H(5) H 0.358(3) 0.555(2) -0.335(3) 0.066(8) Uiso 1.00 calc . . . H(6) H 0.420(2) 0.190(2) -0.011(2) 0.048(6) Uiso 1.00 calc . . . H(7) H 0.495(2) 0.017(2) 0.150(2) 0.048(6) Uiso 1.00 calc . . . H(8) H 0.901(3) -0.005(2) 0.382(2) 0.051(7) Uiso 1.00 calc . . . H(9) H 0.836(3) 0.187(2) -0.098(3) 0.075(9) Uiso 1.00 calc . . . H(10) H 1.021(3) 0.060(3) -0.134(3) 0.080(9) Uiso 1.00 calc . . . H(11) H 1.242(3) 0.067(3) -0.031(3) 0.086(9) Uiso 1.00 calc . . . H(12) H 1.269(3) 0.199(3) 0.119(3) 0.079(9) Uiso 1.00 calc . . . H(13) H 1.075(3) 0.331(3) 0.163(3) 0.078(9) Uiso 1.00 calc . . . H(14) H 0.711(3) -0.267(3) 0.393(3) 0.065(8) Uiso 1.00 calc . . . H(15) H 0.598(3) -0.170(2) 0.239(3) 0.065(8) Uiso 1.00 calc . . . H(16) H 0.588(3) -0.125(2) 0.497(3) 0.070(8) Uiso 1.00 calc . . . H(17) H 0.488(3) -0.021(3) 0.356(3) 0.073(9) Uiso 1.00 calc . . . H(18) H 0.482(3) -0.252(3) 0.379(3) 0.081(10) Uiso 1.00 calc . . . H(19) H 0.391(3) -0.149(3) 0.238(3) 0.09(1) Uiso 1.00 calc . . . H(20) H 0.344(3) -0.092(3) 0.475(4) 0.09(1) Uiso 1.00 calc . . . H(21) H 0.247(4) -0.002(3) 0.317(4) 0.11(1) Uiso 1.00 calc . . . H(22) H 0.240(3) -0.132(3) 0.343(3) 0.10(1) Uiso 1.00 calc . . . H(23) H 0.886(3) -0.235(3) 0.563(3) 0.10(1) Uiso 1.00 calc . . . H(24) H 0.922(3) -0.124(3) 0.546(3) 0.075(9) Uiso 1.00 calc . . . H(25) H 1.107(5) -0.319(4) 0.541(5) 0.17(1) Uiso 1.00 calc . . . H(26) H 1.041(4) -0.241(4) 0.393(4) 0.13(1) Uiso 1.00 calc . . . H(27) H 0.965(7) -0.406(5) 0.453(6) 0.24(1) Uiso 1.00 calc . . . H(28) H 0.89(1) -0.308(9) 0.28(1) 0.412(7) Uiso 1.00 calc . . . H(29) H 1.193(7) -0.483(6) 0.433(7) 0.23(1) Uiso 1.00 calc . . . H(30) H 1.144(6) -0.391(5) 0.331(5) 0.17(1) Uiso 1.00 calc . . . H(31) H 1.087(6) -0.505(5) 0.293(6) 0.21(1) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(1) 0.0417(10) 0.059(1) 0.063(1) -0.0253(9) 0.0257(9) -0.0276(10) O(2) 0.0331(9) 0.061(1) 0.065(1) -0.0178(8) 0.0169(8) -0.0164(9) O(3) 0.0349(8) 0.059(1) 0.050(1) -0.0257(8) 0.0176(8) -0.0118(9) N(1) 0.049(1) 0.059(1) 0.055(1) -0.027(1) 0.023(1) -0.008(1) C(1) 0.036(1) 0.049(1) 0.054(1) -0.022(1) 0.024(1) -0.019(1) C(2) 0.044(1) 0.044(1) 0.053(1) -0.018(1) 0.028(1) -0.015(1) C(3) 0.054(2) 0.056(2) 0.070(2) -0.026(1) 0.030(2) -0.012(2) C(4) 0.074(2) 0.061(2) 0.082(2) -0.032(2) 0.039(2) -0.008(2) C(5) 0.068(2) 0.064(2) 0.068(2) -0.021(2) 0.023(2) 0.004(2) C(6) 0.052(2) 0.057(2) 0.064(2) -0.019(1) 0.022(2) -0.007(2) C(7) 0.042(1) 0.042(1) 0.053(1) -0.014(1) 0.023(1) -0.014(1) C(8) 0.034(1) 0.048(1) 0.049(1) -0.014(1) 0.022(1) -0.021(1) C(9) 0.034(1) 0.052(1) 0.046(1) -0.021(1) 0.023(1) -0.018(1) C(10) 0.033(1) 0.054(1) 0.045(1) -0.020(1) 0.022(1) -0.017(1) C(11) 0.034(1) 0.061(2) 0.046(1) -0.023(1) 0.020(1) -0.016(1) C(12) 0.041(1) 0.062(2) 0.051(1) -0.030(1) 0.026(1) -0.020(1) C(13) 0.044(1) 0.056(2) 0.045(1) -0.023(1) 0.026(1) -0.019(1) C(14) 0.034(1) 0.060(2) 0.043(1) -0.021(1) 0.015(1) -0.012(1) C(15) 0.036(1) 0.054(1) 0.046(1) -0.024(1) 0.022(1) -0.018(1) C(16) 0.034(1) 0.045(1) 0.045(1) -0.015(1) 0.021(1) -0.012(1) C(17) 0.039(1) 0.042(1) 0.054(1) -0.019(1) 0.025(1) -0.012(1) C(18) 0.046(2) 0.073(2) 0.083(2) -0.033(1) 0.036(2) -0.039(2) C(19) 0.060(2) 0.073(2) 0.089(2) -0.034(2) 0.046(2) -0.046(2) C(20) 0.049(2) 0.066(2) 0.078(2) -0.021(1) 0.040(2) -0.023(2) C(21) 0.044(2) 0.088(2) 0.102(2) -0.036(2) 0.045(2) -0.042(2) C(22) 0.046(2) 0.065(2) 0.081(2) -0.031(1) 0.035(1) -0.031(2) C(23) 0.060(2) 0.056(2) 0.060(2) -0.031(1) 0.032(2) -0.015(1) C(24) 0.069(2) 0.068(2) 0.059(2) -0.042(2) 0.039(2) -0.024(2) C(25) 0.075(2) 0.081(2) 0.076(2) -0.048(2) 0.047(2) -0.031(2) C(26) 0.078(2) 0.096(3) 0.088(3) -0.051(2) 0.052(2) -0.028(2) C(27) 0.055(2) 0.068(2) 0.053(2) -0.024(2) 0.022(1) -0.007(2) C(28) 0.057(2) 0.085(3) 0.086(3) -0.017(2) 0.029(2) -0.022(2) C(29) 0.131(4) 0.103(3) 0.153(4) -0.059(3) 0.096(4) -0.060(3) C(30) 0.117(4) 0.113(4) 0.186(6) -0.045(3) 0.099(4) -0.077(4) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(1) 1.427(3) 1_555 1_555 yes O(2) C(8) 1.235(3) 1_555 1_555 yes O(3) C(15) 1.396(3) 1_555 1_555 yes O(3) C(16) 1.372(3) 1_555 1_555 yes N(1) C(13) 1.378(3) 1_555 1_555 yes N(1) C(23) 1.461(3) 1_555 1_555 yes N(1) C(27) 1.464(3) 1_555 1_555 yes C(1) C(2) 1.536(3) 1_555 1_555 yes C(1) C(16) 1.493(3) 1_555 1_555 yes C(1) C(17) 1.535(3) 1_555 1_555 yes C(2) C(3) 1.392(4) 1_555 1_555 yes C(2) C(7) 1.400(3) 1_555 1_555 yes C(3) C(4) 1.377(4) 1_555 1_555 yes C(4) C(5) 1.383(4) 1_555 1_555 yes C(5) C(6) 1.370(4) 1_555 1_555 yes C(6) C(7) 1.399(4) 1_555 1_555 yes C(7) C(8) 1.479(3) 1_555 1_555 yes C(8) C(9) 1.446(3) 1_555 1_555 yes C(9) C(10) 1.438(3) 1_555 1_555 yes C(9) C(16) 1.348(3) 1_555 1_555 yes C(10) C(11) 1.395(3) 1_555 1_555 yes C(10) C(15) 1.386(3) 1_555 1_555 yes C(11) C(12) 1.371(4) 1_555 1_555 yes C(12) C(13) 1.425(3) 1_555 1_555 yes C(13) C(14) 1.404(3) 1_555 1_555 yes C(14) C(15) 1.372(3) 1_555 1_555 yes C(17) C(18) 1.378(3) 1_555 1_555 yes C(17) C(22) 1.372(3) 1_555 1_555 yes C(18) C(19) 1.379(4) 1_555 1_555 yes C(19) C(20) 1.367(4) 1_555 1_555 yes C(20) C(21) 1.370(4) 1_555 1_555 yes C(21) C(22) 1.384(4) 1_555 1_555 yes C(23) C(24) 1.517(4) 1_555 1_555 yes C(24) C(25) 1.518(4) 1_555 1_555 yes C(25) C(26) 1.518(4) 1_555 1_555 yes C(27) C(28) 1.522(4) 1_555 1_555 yes C(28) C(29) 1.485(6) 1_555 1_555 yes C(29) C(30) 1.533(6) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) O(1) H(1) 106(2) 1_555 1_555 1_555 no C(15) O(3) C(16) 105.7(2) 1_555 1_555 1_555 yes C(13) N(1) C(23) 121.1(2) 1_555 1_555 1_555 yes C(13) N(1) C(27) 120.8(2) 1_555 1_555 1_555 yes C(23) N(1) C(27) 117.8(2) 1_555 1_555 1_555 yes O(1) C(1) C(2) 110.9(2) 1_555 1_555 1_555 yes O(1) C(1) C(16) 111.2(2) 1_555 1_555 1_555 yes O(1) C(1) C(17) 107.2(2) 1_555 1_555 1_555 yes C(2) C(1) C(16) 108.4(2) 1_555 1_555 1_555 yes C(2) C(1) C(17) 109.4(2) 1_555 1_555 1_555 yes C(16) C(1) C(17) 109.8(2) 1_555 1_555 1_555 yes C(1) C(2) C(3) 118.1(2) 1_555 1_555 1_555 yes C(1) C(2) C(7) 123.4(2) 1_555 1_555 1_555 yes C(3) C(2) C(7) 118.5(2) 1_555 1_555 1_555 yes C(2) C(3) C(4) 121.1(3) 1_555 1_555 1_555 yes C(2) C(3) H(2) 117(1) 1_555 1_555 1_555 no C(4) C(3) H(2) 121(1) 1_555 1_555 1_555 no C(3) C(4) C(5) 120.3(3) 1_555 1_555 1_555 yes C(3) C(4) H(3) 119(1) 1_555 1_555 1_555 no C(5) C(4) H(3) 120(1) 1_555 1_555 1_555 no C(4) C(5) C(6) 119.6(3) 1_555 1_555 1_555 yes C(4) C(5) H(4) 122(1) 1_555 1_555 1_555 no C(6) C(5) H(4) 118(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 120.9(3) 1_555 1_555 1_555 yes C(5) C(6) H(5) 122(1) 1_555 1_555 1_555 no C(7) C(6) H(5) 116(1) 1_555 1_555 1_555 no C(2) C(7) C(6) 119.6(3) 1_555 1_555 1_555 yes C(2) C(7) C(8) 122.2(2) 1_555 1_555 1_555 yes C(6) C(7) C(8) 118.2(2) 1_555 1_555 1_555 yes O(2) C(8) C(7) 122.2(2) 1_555 1_555 1_555 yes O(2) C(8) C(9) 121.9(2) 1_555 1_555 1_555 yes C(7) C(8) C(9) 115.8(2) 1_555 1_555 1_555 yes C(8) C(9) C(10) 132.2(2) 1_555 1_555 1_555 yes C(8) C(9) C(16) 120.8(2) 1_555 1_555 1_555 yes C(10) C(9) C(16) 107.0(2) 1_555 1_555 1_555 yes C(9) C(10) C(11) 137.2(2) 1_555 1_555 1_555 yes C(9) C(10) C(15) 105.6(2) 1_555 1_555 1_555 yes C(11) C(10) C(15) 117.1(2) 1_555 1_555 1_555 yes C(10) C(11) C(12) 119.4(2) 1_555 1_555 1_555 yes C(10) C(11) H(6) 119(1) 1_555 1_555 1_555 no C(12) C(11) H(6) 121(1) 1_555 1_555 1_555 no C(11) C(12) C(13) 122.7(2) 1_555 1_555 1_555 yes C(11) C(12) H(7) 116(1) 1_555 1_555 1_555 no C(13) C(12) H(7) 120(1) 1_555 1_555 1_555 no N(1) C(13) C(12) 120.4(2) 1_555 1_555 1_555 yes N(1) C(13) C(14) 121.9(2) 1_555 1_555 1_555 yes C(12) C(13) C(14) 117.7(2) 1_555 1_555 1_555 yes C(13) C(14) C(15) 117.4(2) 1_555 1_555 1_555 yes C(13) C(14) H(8) 123(1) 1_555 1_555 1_555 no C(15) C(14) H(8) 118(1) 1_555 1_555 1_555 no O(3) C(15) C(10) 110.0(2) 1_555 1_555 1_555 yes O(3) C(15) C(14) 124.5(2) 1_555 1_555 1_555 yes C(10) C(15) C(14) 125.5(2) 1_555 1_555 1_555 yes O(3) C(16) C(1) 119.0(2) 1_555 1_555 1_555 yes O(3) C(16) C(9) 111.7(2) 1_555 1_555 1_555 yes C(1) C(16) C(9) 129.2(2) 1_555 1_555 1_555 yes C(1) C(17) C(18) 120.1(2) 1_555 1_555 1_555 yes C(1) C(17) C(22) 121.5(2) 1_555 1_555 1_555 yes C(18) C(17) C(22) 118.3(2) 1_555 1_555 1_555 yes C(17) C(18) C(19) 121.2(3) 1_555 1_555 1_555 yes C(17) C(18) H(9) 119(1) 1_555 1_555 1_555 no C(19) C(18) H(9) 119(1) 1_555 1_555 1_555 no C(18) C(19) C(20) 120.3(3) 1_555 1_555 1_555 yes C(18) C(19) H(10) 118(1) 1_555 1_555 1_555 no C(20) C(19) H(10) 121(1) 1_555 1_555 1_555 no C(19) C(20) C(21) 119.0(3) 1_555 1_555 1_555 yes C(19) C(20) H(11) 121(1) 1_555 1_555 1_555 no C(21) C(20) H(11) 119(1) 1_555 1_555 1_555 no C(20) C(21) C(22) 120.9(3) 1_555 1_555 1_555 yes C(20) C(21) H(12) 117(1) 1_555 1_555 1_555 no C(22) C(21) H(12) 121(1) 1_555 1_555 1_555 no C(17) C(22) C(21) 120.4(3) 1_555 1_555 1_555 yes C(17) C(22) H(13) 118(1) 1_555 1_555 1_555 no C(21) C(22) H(13) 121(1) 1_555 1_555 1_555 no N(1) C(23) C(24) 114.3(2) 1_555 1_555 1_555 yes N(1) C(23) H(14) 109(1) 1_555 1_555 1_555 no N(1) C(23) H(15) 109(1) 1_555 1_555 1_555 no C(24) C(23) H(14) 108(1) 1_555 1_555 1_555 no C(24) C(23) H(15) 107(1) 1_555 1_555 1_555 no H(14) C(23) H(15) 106(1) 1_555 1_555 1_555 no C(23) C(24) C(25) 112.7(2) 1_555 1_555 1_555 yes C(23) C(24) H(16) 108(1) 1_555 1_555 1_555 no C(23) C(24) H(17) 109(1) 1_555 1_555 1_555 no C(25) C(24) H(16) 111(1) 1_555 1_555 1_555 no C(25) C(24) H(17) 110(1) 1_555 1_555 1_555 no H(16) C(24) H(17) 103(2) 1_555 1_555 1_555 no C(24) C(25) C(26) 112.8(3) 1_555 1_555 1_555 yes C(24) C(25) H(18) 107(1) 1_555 1_555 1_555 no C(24) C(25) H(19) 103(1) 1_555 1_555 1_555 no C(26) C(25) H(18) 115(1) 1_555 1_555 1_555 no C(26) C(25) H(19) 110(1) 1_555 1_555 1_555 no H(18) C(25) H(19) 106(2) 1_555 1_555 1_555 no C(25) C(26) H(20) 111(1) 1_555 1_555 1_555 no C(25) C(26) H(21) 109(1) 1_555 1_555 1_555 no C(25) C(26) H(22) 108(1) 1_555 1_555 1_555 no H(20) C(26) H(21) 109(2) 1_555 1_555 1_555 no H(20) C(26) H(22) 110(2) 1_555 1_555 1_555 no H(21) C(26) H(22) 108(2) 1_555 1_555 1_555 no N(1) C(27) C(28) 114.7(3) 1_555 1_555 1_555 yes N(1) C(27) H(23) 106(1) 1_555 1_555 1_555 no N(1) C(27) H(24) 109(1) 1_555 1_555 1_555 no C(28) C(27) H(23) 112(1) 1_555 1_555 1_555 no C(28) C(27) H(24) 108(1) 1_555 1_555 1_555 no H(23) C(27) H(24) 105(2) 1_555 1_555 1_555 no C(27) C(28) C(29) 114.7(3) 1_555 1_555 1_555 yes C(27) C(28) H(25) 114(2) 1_555 1_555 1_555 no C(27) C(28) H(26) 129(2) 1_555 1_555 1_555 no C(29) C(28) H(25) 103(2) 1_555 1_555 1_555 no C(29) C(28) H(26) 93(2) 1_555 1_555 1_555 no H(25) C(28) H(26) 97(3) 1_555 1_555 1_555 no C(28) C(29) C(30) 112.8(5) 1_555 1_555 1_555 yes C(28) C(29) H(27) 97(3) 1_555 1_555 1_555 no C(28) C(29) H(28) 103(5) 1_555 1_555 1_555 no C(30) C(29) H(27) 115(3) 1_555 1_555 1_555 no C(30) C(29) H(28) 106(5) 1_555 1_555 1_555 no H(27) C(29) H(28) 119(6) 1_555 1_555 1_555 no C(29) C(30) H(29) 111(3) 1_555 1_555 1_555 no C(29) C(30) H(30) 108(2) 1_555 1_555 1_555 no C(29) C(30) H(31) 117(3) 1_555 1_555 1_555 no H(29) C(30) H(30) 82(4) 1_555 1_555 1_555 no H(29) C(30) H(31) 108(4) 1_555 1_555 1_555 no H(30) C(30) H(31) 122(4) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ #===============================================END data_3d _database_code_CSD 172462 #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_formula_sum 'C34 H39 N O3 ' _chemical_formula_weight 509.69 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _cell_length_a 9.061(1) _cell_length_b 20.227(2) _cell_length_c 8.751(1) _cell_angle_alpha 101.52(1) _cell_angle_beta 114.30(1) _cell_angle_gamma 87.75(1) _cell_volume 1430.6(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.183 _diffrn_radiation_type 'Mo K¥a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.2 _cell_measurement_theta_max 12.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_F_000 548.00 _exptl_absorpt_coefficient_mu 0.074 _exptl_crystal_description 'prismatic' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.100 _exptl_crystal_colour 'yellow' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method ¥w-2¥q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.966 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_radiation_monochromator graphite _diffrn_reflns_number 5385 _reflns_number_total 5036 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_limit_h_min -0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.843 _refine_ls_number_reflns 2082 _refine_ls_number_parameters 448 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[¥s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0753 _refine_ls_shift/su_mean 0.0041 _refine_diff_density_min -0.20 _refine_diff_density_max 0.27 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 1.1476(5) 0.3653(2) 0.8526(5) 0.055(1) Uani 1.00 d . . . O(2) O 0.9408(6) 0.1894(2) 0.2536(6) 0.076(2) Uani 1.00 d . . . O(3) O 0.9546(5) 0.2443(2) 0.7961(5) 0.049(1) Uani 1.00 d . . . N(1) N 0.7992(7) 0.0210(2) 0.8176(7) 0.060(2) Uani 1.00 d . . . C(1) C 1.0141(7) 0.3419(3) 0.6959(8) 0.048(2) Uani 1.00 d . . . C(2) C 1.0493(7) 0.3530(3) 0.5441(8) 0.049(2) Uani 1.00 d . . . C(3) C 1.1044(8) 0.4172(3) 0.5520(9) 0.055(2) Uani 1.00 d . . . C(4) C 1.1371(9) 0.4318(4) 0.423(1) 0.065(3) Uani 1.00 d . . . C(5) C 1.1184(9) 0.3816(4) 0.281(1) 0.062(3) Uani 1.00 d . . . C(6) C 1.0607(8) 0.3181(4) 0.2677(9) 0.055(2) Uani 1.00 d . . . C(7) C 1.0277(7) 0.3028(3) 0.4000(8) 0.049(2) Uani 1.00 d . . . C(8) C 0.9706(7) 0.2322(3) 0.3838(8) 0.050(2) Uani 1.00 d . . . C(9) C 0.9549(7) 0.2176(3) 0.5324(7) 0.045(2) Uani 1.00 d . . . C(10) C 0.9118(7) 0.1564(3) 0.5708(7) 0.044(2) Uani 1.00 d . . . C(11) C 0.8742(8) 0.0893(3) 0.4909(9) 0.055(2) Uani 1.00 d . . . C(12) C 0.8389(9) 0.0450(4) 0.5746(9) 0.065(2) Uani 1.00 d . . . C(13) C 0.8387(7) 0.0657(3) 0.7381(8) 0.051(2) Uani 1.00 d . . . C(14) C 0.8800(8) 0.1340(3) 0.8193(8) 0.047(2) Uani 1.00 d . . . C(15) C 0.9150(7) 0.1758(3) 0.7324(8) 0.045(2) Uani 1.00 d . . . C(16) C 0.9781(7) 0.2676(3) 0.6701(7) 0.045(2) Uani 1.00 d . . . C(17) C 0.8687(7) 0.3809(3) 0.7008(7) 0.042(2) Uani 1.00 d . . . C(18) C 0.7206(9) 0.3690(4) 0.5614(9) 0.065(2) Uani 1.00 d . . . C(19) C 0.5855(10) 0.4038(4) 0.561(1) 0.077(3) Uani 1.00 d . . . C(20) C 0.5965(9) 0.4516(4) 0.701(1) 0.067(3) Uani 1.00 d . . . C(21) C 0.742(1) 0.4646(4) 0.838(1) 0.067(3) Uani 1.00 d . . . C(22) C 0.8759(9) 0.4293(3) 0.8390(9) 0.059(2) Uani 1.00 d . . . C(23) C 0.794(1) -0.0525(4) 0.759(1) 0.073(3) Uani 1.00 d . . . C(24) C 0.632(1) -0.0843(4) 0.645(1) 0.097(4) Uani 1.00 d . . . C(25) C 0.653(2) -0.1622(6) 0.600(2) 0.154(6) Uani 1.00 d . . . C(26) C 0.532(2) -0.2023(6) 0.575(3) 0.233(9) Uani 1.00 d . . . C(27) C 0.7548(9) 0.0455(4) 0.958(1) 0.062(3) Uani 1.00 d . . . C(28) C 0.580(2) 0.0738(7) 0.883(2) 0.162(7) Uani 1.00 d . . . C(29) C 0.516(2) 0.1023(7) 0.983(2) 0.192(8) Uani 1.00 d . . . C(30) C 0.332(1) 0.1231(5) 0.883(2) 0.142(5) Uani 1.00 d . . . C(31) C 1.2920(9) 0.3282(4) 0.872(1) 0.070(3) Uani 1.00 d . . . C(32) C 1.436(1) 0.3673(5) 1.019(1) 0.103(3) Uani 1.00 d . . . C(33) C 1.589(1) 0.3272(6) 1.071(1) 0.132(4) Uani 1.00 d . . . C(34) C 1.631(1) 0.2928(6) 0.934(2) 0.139(5) Uani 1.00 d . . . H(1) H 1.129(6) 0.452(2) 0.662(6) 0.04(1) Uiso 1.00 calc . . . H(2) H 1.173(7) 0.473(3) 0.430(8) 0.07(2) Uiso 1.00 calc . . . H(3) H 1.136(6) 0.390(3) 0.191(7) 0.05(2) Uiso 1.00 calc . . . H(4) H 1.049(6) 0.282(3) 0.180(7) 0.05(2) Uiso 1.00 calc . . . H(5) H 0.871(6) 0.073(2) 0.374(7) 0.04(1) Uiso 1.00 calc . . . H(6) H 0.823(7) 0.000(3) 0.516(7) 0.07(2) Uiso 1.00 calc . . . H(7) H 0.878(6) 0.154(3) 0.924(7) 0.05(2) Uiso 1.00 calc . . . H(8) H 0.716(6) 0.333(3) 0.449(7) 0.06(2) Uiso 1.00 calc . . . H(9) H 0.458(9) 0.392(4) 0.453(10) 0.12(2) Uiso 1.00 calc . . . H(10) H 0.508(7) 0.477(3) 0.731(7) 0.06(2) Uiso 1.00 calc . . . H(11) H 0.749(7) 0.493(3) 0.942(8) 0.07(2) Uiso 1.00 calc . . . H(12) H 0.973(8) 0.437(3) 0.921(9) 0.08(2) Uiso 1.00 calc . . . H(13) H 0.861(7) -0.062(3) 0.702(8) 0.06(2) Uiso 1.00 calc . . . H(14) H 0.849(10) -0.078(4) 0.87(1) 0.13(1) Uiso 1.00 calc . . . H(15) H 0.59(1) -0.056(5) 0.54(1) 0.17(1) Uiso 1.00 calc . . . H(16) H 0.566(7) -0.073(3) 0.706(8) 0.06(2) Uiso 1.00 calc . . . H(17) H 0.72(1) -0.167(6) 0.52(2) 0.205(9) Uiso 1.00 calc . . . H(18) H 0.547(7) -0.152(3) 0.503(7) 0.04(2) Uiso 1.00 calc . . . H(19) H 0.4650 -0.1826 0.6042 0.2921 Uiso 1.00 calc . . . H(20) H 0.4984 -0.2294 0.4595 0.2921 Uiso 1.00 calc . . . H(21) H 0.5925 -0.2372 0.6479 0.2921 Uiso 1.00 calc . . . H(22) H 0.738(6) 0.010(3) 0.992(7) 0.05(2) Uiso 1.00 calc . . . H(23) H 0.864(9) 0.081(4) 1.076(10) 0.12(2) Uiso 1.00 calc . . . H(24) H 0.574(8) 0.098(3) 0.816(9) 0.08(2) Uiso 1.00 calc . . . H(25) H 0.452(3) 0.058(1) 0.834(3) -0.038(6) Uiso 1.00 calc . . . H(26) H 0.5936 0.1435 1.0466 0.2379 Uiso 1.00 calc . . . H(27) H 0.5339 0.0766 1.0685 0.2379 Uiso 1.00 calc . . . H(28) H 0.3276 0.1485 0.7999 0.1702 Uiso 1.00 calc . . . H(29) H 0.2932 0.1476 0.9592 0.1702 Uiso 1.00 calc . . . H(30) H 0.2677 0.0818 0.8229 0.1702 Uiso 1.00 calc . . . H(31) H 1.337(8) 0.306(4) 0.772(9) 0.11(2) Uiso 1.00 calc . . . H(32) H 1.297(9) 0.289(4) 0.918(9) 0.10(2) Uiso 1.00 calc . . . H(33) H 1.41(1) 0.373(5) 1.11(1) 0.15(1) Uiso 1.00 calc . . . H(34) H 1.49(3) 0.40(1) 0.96(3) 0.501(4) Uiso 1.00 calc . . . H(35) H 1.6754 0.3586 1.1457 0.1593 Uiso 1.00 calc . . . H(36) H 1.5766 0.2945 1.1285 0.1593 Uiso 1.00 calc . . . H(37) H 1.5452 0.2614 0.8576 0.1658 Uiso 1.00 calc . . . H(38) H 1.7274 0.2706 0.9817 0.1658 Uiso 1.00 calc . . . H(39) H 1.6453 0.3252 0.8759 0.1658 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(1) 0.057(3) 0.050(3) 0.050(3) -0.002(2) 0.016(2) 0.002(2) O(2) 0.115(4) 0.062(3) 0.051(3) -0.012(3) 0.040(3) -0.004(2) O(3) 0.069(3) 0.040(3) 0.043(2) -0.001(2) 0.029(2) 0.004(2) N(1) 0.086(4) 0.038(3) 0.068(4) -0.004(3) 0.041(3) 0.013(3) C(1) 0.048(4) 0.041(4) 0.049(4) -0.001(3) 0.013(3) 0.009(3) C(2) 0.050(4) 0.049(4) 0.052(4) 0.001(3) 0.024(3) 0.015(3) C(3) 0.059(5) 0.051(4) 0.058(5) -0.002(3) 0.026(4) 0.013(4) C(4) 0.064(5) 0.059(5) 0.094(6) 0.004(4) 0.046(5) 0.032(5) C(5) 0.068(5) 0.069(5) 0.072(6) 0.008(4) 0.043(4) 0.033(5) C(6) 0.052(4) 0.066(5) 0.047(4) 0.002(4) 0.021(4) 0.011(4) C(7) 0.055(4) 0.055(4) 0.042(4) 0.007(3) 0.022(3) 0.015(3) C(8) 0.052(4) 0.053(4) 0.046(4) -0.001(3) 0.020(3) 0.011(3) C(9) 0.055(4) 0.038(3) 0.039(3) 0.000(3) 0.018(3) 0.004(3) C(10) 0.056(4) 0.040(4) 0.040(4) 0.001(3) 0.025(3) 0.004(3) C(11) 0.076(5) 0.044(4) 0.049(4) 0.000(3) 0.032(4) 0.003(3) C(12) 0.085(6) 0.041(4) 0.063(5) -0.006(4) 0.030(4) -0.003(4) C(13) 0.058(4) 0.045(4) 0.048(4) 0.000(3) 0.020(3) 0.010(3) C(14) 0.053(4) 0.044(4) 0.044(4) -0.004(3) 0.020(3) 0.003(3) C(15) 0.051(4) 0.031(3) 0.048(4) -0.005(3) 0.020(3) 0.000(3) C(16) 0.053(4) 0.044(4) 0.044(4) 0.007(3) 0.023(3) 0.014(3) C(17) 0.036(4) 0.044(4) 0.045(4) 0.003(3) 0.014(3) 0.012(3) C(18) 0.063(5) 0.066(5) 0.063(5) 0.016(4) 0.027(4) 0.007(4) C(19) 0.054(5) 0.082(6) 0.085(6) 0.008(4) 0.019(5) 0.013(5) C(20) 0.053(5) 0.073(5) 0.078(6) 0.006(4) 0.028(5) 0.014(4) C(21) 0.081(6) 0.051(5) 0.076(6) 0.016(4) 0.042(5) 0.009(4) C(22) 0.066(5) 0.046(4) 0.059(5) 0.005(4) 0.025(4) 0.003(4) C(23) 0.097(7) 0.048(5) 0.092(6) 0.005(4) 0.051(6) 0.025(4) C(24) 0.112(8) 0.064(6) 0.120(8) -0.026(5) 0.068(7) -0.019(5) C(25) 0.17(1) 0.066(7) 0.24(2) -0.040(8) 0.12(1) -0.038(9) C(26) 0.28(2) 0.062(8) 0.44(3) -0.016(10) 0.25(2) 0.01(1) C(27) 0.078(6) 0.050(5) 0.079(5) -0.001(4) 0.047(5) 0.024(4) C(28) 0.23(2) 0.15(1) 0.26(2) 0.10(1) 0.22(1) 0.14(1) C(29) 0.27(2) 0.16(1) 0.22(2) 0.02(1) 0.15(2) 0.09(1) C(30) 0.078(7) 0.139(9) 0.24(1) 0.043(7) 0.072(8) 0.094(9) C(31) 0.050(5) 0.062(5) 0.087(6) 0.022(4) 0.022(4) 0.007(4) C(32) 0.058(6) 0.135(9) 0.078(6) 0.019(5) 0.008(5) -0.018(6) C(33) 0.073(6) 0.20(1) 0.075(7) 0.044(7) 0.010(5) -0.013(7) C(34) 0.112(8) 0.145(10) 0.16(1) 0.022(7) 0.060(8) 0.025(8) O(1) 0.0417(10) 0.059(1) 0.063(1) -0.0253(9) 0.0257(9) -0.0276(10) O(2) 0.0331(9) 0.061(1) 0.065(1) -0.0178(8) 0.0169(8) -0.0164(9) O(3) 0.0349(8) 0.059(1) 0.050(1) -0.0257(8) 0.0176(8) -0.0118(9) N(1) 0.049(1) 0.059(1) 0.055(1) -0.027(1) 0.023(1) -0.008(1) C(1) 0.036(1) 0.049(1) 0.054(1) -0.022(1) 0.024(1) -0.019(1) C(2) 0.044(1) 0.044(1) 0.053(1) -0.018(1) 0.028(1) -0.015(1) C(3) 0.054(2) 0.056(2) 0.070(2) -0.026(1) 0.030(2) -0.012(2) C(4) 0.074(2) 0.061(2) 0.082(2) -0.032(2) 0.039(2) -0.008(2) C(5) 0.068(2) 0.064(2) 0.068(2) -0.021(2) 0.023(2) 0.004(2) C(6) 0.052(2) 0.057(2) 0.064(2) -0.019(1) 0.022(2) -0.007(2) C(7) 0.042(1) 0.042(1) 0.053(1) -0.014(1) 0.023(1) -0.014(1) C(8) 0.034(1) 0.048(1) 0.049(1) -0.014(1) 0.022(1) -0.021(1) C(9) 0.034(1) 0.052(1) 0.046(1) -0.021(1) 0.023(1) -0.018(1) C(10) 0.033(1) 0.054(1) 0.045(1) -0.020(1) 0.022(1) -0.017(1) C(11) 0.034(1) 0.061(2) 0.046(1) -0.023(1) 0.020(1) -0.016(1) C(12) 0.041(1) 0.062(2) 0.051(1) -0.030(1) 0.026(1) -0.020(1) C(13) 0.044(1) 0.056(2) 0.045(1) -0.023(1) 0.026(1) -0.019(1) C(14) 0.034(1) 0.060(2) 0.043(1) -0.021(1) 0.015(1) -0.012(1) C(15) 0.036(1) 0.054(1) 0.046(1) -0.024(1) 0.022(1) -0.018(1) C(16) 0.034(1) 0.045(1) 0.045(1) -0.015(1) 0.021(1) -0.012(1) C(17) 0.039(1) 0.042(1) 0.054(1) -0.019(1) 0.025(1) -0.012(1) C(18) 0.046(2) 0.073(2) 0.083(2) -0.033(1) 0.036(2) -0.039(2) C(19) 0.060(2) 0.073(2) 0.089(2) -0.034(2) 0.046(2) -0.046(2) C(20) 0.049(2) 0.066(2) 0.078(2) -0.021(1) 0.040(2) -0.023(2) C(21) 0.044(2) 0.088(2) 0.102(2) -0.036(2) 0.045(2) -0.042(2) C(22) 0.046(2) 0.065(2) 0.081(2) -0.031(1) 0.035(1) -0.031(2) C(23) 0.060(2) 0.056(2) 0.060(2) -0.031(1) 0.032(2) -0.015(1) C(24) 0.069(2) 0.068(2) 0.059(2) -0.042(2) 0.039(2) -0.024(2) C(25) 0.075(2) 0.081(2) 0.076(2) -0.048(2) 0.047(2) -0.031(2) C(26) 0.078(2) 0.096(3) 0.088(3) -0.051(2) 0.052(2) -0.028(2) C(27) 0.055(2) 0.068(2) 0.053(2) -0.024(2) 0.022(1) -0.007(2) C(28) 0.057(2) 0.085(3) 0.086(3) -0.017(2) 0.029(2) -0.022(2) C(29) 0.131(4) 0.103(3) 0.153(4) -0.059(3) 0.096(4) -0.060(3) C(30) 0.117(4) 0.113(4) 0.186(6) -0.045(3) 0.099(4) -0.077(4) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(1) 1.410(6) 1_555 1_555 yes O(1) C(31) 1.447(8) 1_555 1_555 yes O(2) C(8) 1.222(7) 1_555 1_555 yes O(3) C(15) 1.387(6) 1_555 1_555 yes O(3) C(16) 1.376(6) 1_555 1_555 yes N(1) C(13) 1.383(7) 1_555 1_555 yes N(1) C(23) 1.469(9) 1_555 1_555 yes N(1) C(27) 1.440(8) 1_555 1_555 yes C(1) C(2) 1.546(8) 1_555 1_555 yes C(1) C(16) 1.503(8) 1_555 1_555 yes C(1) C(17) 1.520(8) 1_555 1_555 yes C(2) C(3) 1.388(8) 1_555 1_555 yes C(2) C(7) 1.401(8) 1_555 1_555 yes C(3) C(4) 1.369(9) 1_555 1_555 yes C(4) C(5) 1.392(10) 1_555 1_555 yes C(5) C(6) 1.372(9) 1_555 1_555 yes C(6) C(7) 1.400(8) 1_555 1_555 yes C(7) C(8) 1.498(8) 1_555 1_555 yes C(8) C(9) 1.451(8) 1_555 1_555 yes C(9) C(10) 1.453(8) 1_555 1_555 yes C(9) C(16) 1.356(7) 1_555 1_555 yes C(10) C(11) 1.380(8) 1_555 1_555 yes C(10) C(15) 1.378(7) 1_555 1_555 yes C(11) C(12) 1.385(9) 1_555 1_555 yes C(12) C(13) 1.409(9) 1_555 1_555 yes C(13) C(14) 1.407(8) 1_555 1_555 yes C(14) C(15) 1.368(8) 1_555 1_555 yes C(17) C(18) 1.381(8) 1_555 1_555 yes C(17) C(22) 1.375(8) 1_555 1_555 yes C(18) C(19) 1.387(9) 1_555 1_555 yes C(19) C(20) 1.371(10) 1_555 1_555 yes C(20) C(21) 1.36(1) 1_555 1_555 yes C(21) C(22) 1.381(10) 1_555 1_555 yes C(23) C(24) 1.48(1) 1_555 1_555 yes C(24) C(25) 1.57(1) 1_555 1_555 yes C(25) C(26) 1.31(1) 1_555 1_555 yes C(27) C(28) 1.58(2) 1_555 1_555 yes C(28) C(29) 1.27(2) 1_555 1_555 yes C(29) C(30) 1.61(2) 1_555 1_555 yes C(31) C(32) 1.51(1) 1_555 1_555 yes C(32) C(33) 1.52(1) 1_555 1_555 yes C(33) C(34) 1.44(1) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) O(1) C(31) 113.6(5) 1_555 1_555 1_555 yes C(15) O(3) C(16) 105.1(4) 1_555 1_555 1_555 yes C(13) N(1) C(23) 122.0(6) 1_555 1_555 1_555 yes C(13) N(1) C(27) 120.5(5) 1_555 1_555 1_555 yes C(23) N(1) C(27) 117.4(6) 1_555 1_555 1_555 yes O(1) C(1) C(2) 110.6(5) 1_555 1_555 1_555 yes O(1) C(1) C(16) 111.1(5) 1_555 1_555 1_555 yes O(1) C(1) C(17) 107.6(5) 1_555 1_555 1_555 yes C(2) C(1) C(16) 107.5(5) 1_555 1_555 1_555 yes C(2) C(1) C(17) 110.5(5) 1_555 1_555 1_555 yes C(16) C(1) C(17) 109.6(5) 1_555 1_555 1_555 yes C(1) C(2) C(3) 117.3(6) 1_555 1_555 1_555 yes C(1) C(2) C(7) 124.2(5) 1_555 1_555 1_555 yes C(3) C(2) C(7) 118.5(6) 1_555 1_555 1_555 yes C(2) C(3) C(4) 121.3(7) 1_555 1_555 1_555 yes C(2) C(3) H(1) 118(2) 1_555 1_555 1_555 no C(4) C(3) H(1) 120(2) 1_555 1_555 1_555 no C(3) C(4) C(5) 120.3(7) 1_555 1_555 1_555 yes C(3) C(4) H(2) 119(4) 1_555 1_555 1_555 no C(5) C(4) H(2) 119(4) 1_555 1_555 1_555 no C(4) C(5) C(6) 119.5(7) 1_555 1_555 1_555 yes C(4) C(5) H(3) 122(3) 1_555 1_555 1_555 no C(6) C(5) H(3) 118(3) 1_555 1_555 1_555 no C(5) C(6) C(7) 120.4(7) 1_555 1_555 1_555 yes C(5) C(6) H(4) 124(3) 1_555 1_555 1_555 no C(7) C(6) H(4) 114(3) 1_555 1_555 1_555 no C(2) C(7) C(6) 119.9(6) 1_555 1_555 1_555 yes C(2) C(7) C(8) 121.4(5) 1_555 1_555 1_555 yes C(6) C(7) C(8) 118.7(6) 1_555 1_555 1_555 yes O(2) C(8) C(7) 121.7(6) 1_555 1_555 1_555 yes O(2) C(8) C(9) 122.2(6) 1_555 1_555 1_555 yes C(7) C(8) C(9) 116.1(5) 1_555 1_555 1_555 yes C(8) C(9) C(10) 133.0(5) 1_555 1_555 1_555 yes C(8) C(9) C(16) 120.4(6) 1_555 1_555 1_555 yes C(10) C(9) C(16) 106.6(5) 1_555 1_555 1_555 yes C(9) C(10) C(11) 137.1(6) 1_555 1_555 1_555 yes C(9) C(10) C(15) 104.9(5) 1_555 1_555 1_555 yes C(11) C(10) C(15) 118.0(6) 1_555 1_555 1_555 yes C(10) C(11) C(12) 119.0(6) 1_555 1_555 1_555 yes C(10) C(11) H(5) 121(2) 1_555 1_555 1_555 no C(12) C(11) H(5) 120(2) 1_555 1_555 1_555 no C(11) C(12) C(13) 122.6(6) 1_555 1_555 1_555 yes C(11) C(12) H(6) 113(3) 1_555 1_555 1_555 no C(13) C(12) H(6) 123(3) 1_555 1_555 1_555 no N(1) C(13) C(12) 121.7(6) 1_555 1_555 1_555 yes N(1) C(13) C(14) 120.5(5) 1_555 1_555 1_555 yes C(12) C(13) C(14) 117.9(6) 1_555 1_555 1_555 yes C(13) C(14) C(15) 117.6(6) 1_555 1_555 1_555 yes C(13) C(14) H(7) 124(3) 1_555 1_555 1_555 no C(15) C(14) H(7) 117(3) 1_555 1_555 1_555 no O(3) C(15) C(10) 111.5(5) 1_555 1_555 1_555 yes O(3) C(15) C(14) 123.5(5) 1_555 1_555 1_555 yes C(10) C(15) C(14) 125.0(5) 1_555 1_555 1_555 yes O(3) C(16) C(1) 118.4(5) 1_555 1_555 1_555 yes O(3) C(16) C(9) 111.9(5) 1_555 1_555 1_555 yes C(1) C(16) C(9) 129.6(6) 1_555 1_555 1_555 yes C(1) C(17) C(18) 120.1(6) 1_555 1_555 1_555 yes C(1) C(17) C(22) 123.2(6) 1_555 1_555 1_555 yes C(18) C(17) C(22) 116.7(6) 1_555 1_555 1_555 yes C(17) C(18) C(19) 121.7(7) 1_555 1_555 1_555 yes C(17) C(18) H(8) 117(2) 1_555 1_555 1_555 no C(19) C(18) H(8) 121(2) 1_555 1_555 1_555 no C(18) C(19) C(20) 120.1(8) 1_555 1_555 1_555 yes C(18) C(19) H(9) 123(3) 1_555 1_555 1_555 no C(20) C(19) H(9) 115(3) 1_555 1_555 1_555 no C(19) C(20) C(21) 118.8(8) 1_555 1_555 1_555 yes C(19) C(20) H(10) 131(3) 1_555 1_555 1_555 no C(21) C(20) H(10) 109(3) 1_555 1_555 1_555 no C(20) C(21) C(22) 120.8(8) 1_555 1_555 1_555 yes C(20) C(21) H(11) 119(3) 1_555 1_555 1_555 no C(22) C(21) H(11) 118(3) 1_555 1_555 1_555 no C(17) C(22) C(21) 121.7(8) 1_555 1_555 1_555 yes C(17) C(22) H(12) 112(4) 1_555 1_555 1_555 no C(21) C(22) H(12) 125(4) 1_555 1_555 1_555 no N(1) C(23) C(24) 115.4(7) 1_555 1_555 1_555 yes N(1) C(23) H(13) 108(3) 1_555 1_555 1_555 no N(1) C(23) H(14) 111(4) 1_555 1_555 1_555 no C(24) C(23) H(13) 108(4) 1_555 1_555 1_555 no C(24) C(23) H(14) 109(4) 1_555 1_555 1_555 no H(13) C(23) H(14) 103(5) 1_555 1_555 1_555 no C(23) C(24) C(25) 107.2(10) 1_555 1_555 1_555 yes C(23) C(24) H(15) 104(5) 1_555 1_555 1_555 no C(23) C(24) H(16) 106(3) 1_555 1_555 1_555 no C(25) C(24) H(15) 118(5) 1_555 1_555 1_555 no C(25) C(24) H(16) 113(3) 1_555 1_555 1_555 no H(15) C(24) H(16) 106(6) 1_555 1_555 1_555 no C(24) C(25) C(26) 116(1) 1_555 1_555 1_555 yes C(24) C(25) H(17) 105(6) 1_555 1_555 1_555 no C(24) C(25) H(18) 74(3) 1_555 1_555 1_555 no C(26) C(25) H(17) 125(6) 1_555 1_555 1_555 no C(26) C(25) H(18) 68(3) 1_555 1_555 1_555 no H(17) C(25) H(18) 92(8) 1_555 1_555 1_555 no C(25) C(26) H(19) 112(1) 1_555 1_555 1_555 no C(25) C(26) H(20) 106(1) 1_555 1_555 1_555 no C(25) C(26) H(21) 100(1) 1_555 1_555 1_555 no H(19) C(26) H(20) 119(2) 1_555 1_555 1_555 no H(19) C(26) H(21) 113(1) 1_555 1_555 1_555 no H(20) C(26) H(21) 101.0(10) 1_555 1_555 1_555 no N(1) C(27) C(28) 107.7(8) 1_555 1_555 1_555 yes N(1) C(27) H(22) 106(3) 1_555 1_555 1_555 no N(1) C(27) H(23) 111(3) 1_555 1_555 1_555 no C(28) C(27) H(22) 102(3) 1_555 1_555 1_555 no C(28) C(27) H(23) 119(3) 1_555 1_555 1_555 no H(22) C(27) H(23) 109(5) 1_555 1_555 1_555 no C(27) C(28) C(29) 120(1) 1_555 1_555 1_555 yes C(27) C(28) H(24) 110(5) 1_555 1_555 1_555 no C(27) C(28) H(25) 141(1) 1_555 1_555 1_555 no C(29) C(28) H(24) 110(5) 1_555 1_555 1_555 no C(29) C(28) H(25) 68(1) 1_555 1_555 1_555 no H(24) C(28) H(25) 99(5) 1_555 1_555 1_555 no C(28) C(29) C(30) 113(1) 1_555 1_555 1_555 yes C(28) C(29) H(26) 99(1) 1_555 1_555 1_555 no C(28) C(29) H(27) 109(1) 1_555 1_555 1_555 no C(30) C(29) H(26) 112(1) 1_555 1_555 1_555 no C(30) C(29) H(27) 116(1) 1_555 1_555 1_555 no H(26) C(29) H(27) 103(1) 1_555 1_555 1_555 no C(29) C(30) H(28) 110.1(9) 1_555 1_555 1_555 no C(29) C(30) H(29) 110(1) 1_555 1_555 1_555 no C(29) C(30) H(30) 107.1(9) 1_555 1_555 1_555 no H(28) C(30) H(29) 110(1) 1_555 1_555 1_555 no H(28) C(30) H(30) 108(1) 1_555 1_555 1_555 no H(29) C(30) H(30) 110.1(10) 1_555 1_555 1_555 no O(1) C(31) C(32) 109.2(6) 1_555 1_555 1_555 yes O(1) C(31) H(31) 128(3) 1_555 1_555 1_555 no O(1) C(31) H(32) 113(4) 1_555 1_555 1_555 no C(32) C(31) H(31) 105(3) 1_555 1_555 1_555 no C(32) C(31) H(32) 97(4) 1_555 1_555 1_555 no H(31) C(31) H(32) 97(5) 1_555 1_555 1_555 no C(31) C(32) C(33) 113.3(8) 1_555 1_555 1_555 yes C(31) C(32) H(33) 103(6) 1_555 1_555 1_555 no C(31) C(32) H(34) 106(11) 1_555 1_555 1_555 no C(33) C(32) H(33) 104(6) 1_555 1_555 1_555 no C(33) C(32) H(34) 90(11) 1_555 1_555 1_555 no H(33) C(32) H(34) 137(13) 1_555 1_555 1_555 no C(32) C(33) C(34) 116.6(9) 1_555 1_555 1_555 yes C(32) C(33) H(35) 106(1) 1_555 1_555 1_555 no C(32) C(33) H(36) 108(1) 1_555 1_555 1_555 no C(34) C(33) H(35) 107.5(10) 1_555 1_555 1_555 no C(34) C(33) H(36) 107(1) 1_555 1_555 1_555 no H(35) C(33) H(36) 110.1(10) 1_555 1_555 1_555 no C(33) C(34) H(37) 108(1) 1_555 1_555 1_555 no C(33) C(34) H(38) 108(1) 1_555 1_555 1_555 no C(33) C(34) H(39) 108(1) 1_555 1_555 1_555 no H(37) C(34) H(38) 110(1) 1_555 1_555 1_555 no H(37) C(34) H(39) 109(1) 1_555 1_555 1_555 no H(38) C(34) H(39) 110(1) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ #===============================================END