Supplementary Material (ESI) for Organic and Biomolecular Chemistry This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _publ_contact_author_name 'Katsuhira Yoshida' _publ_contact_author_address ; Department of Material Science Kochi University Akebono-cho, 2-5-1 Kochi 780-8520 JAPAN ; _publ_contact_author_email KYOSHIDA@CC.KOCHI-U.AC.JP _publ_section_title ; Molecular design of novel non-planar heteropolycyclic fluorophores with bulky substituents: convenient synthesis and solid-state fluorescence characterization ; _publ_section_references ; Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; loop_ _publ_author_name 'Katsuhira Yoshida' 'Yousuke Ooyama' 'Shigeru Watanabe' 'Shintaro Yoshikawa' data_2a _database_code_depnum_ccdc_archive 'CCDC 605725' _audit_creation_date 'Tue Jan 3 09:51:36 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #--------------------------------------------------------------------------- #-- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------------- #-- _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 493.69 _chemical_formula_analytical ? _chemical_formula_sum ' C34 H39 N O2 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_melting_point ? #--------------------------------------------------------------------------- #-- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 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 14.321(2) _cell_length_b 11.583(3) _cell_length_c 17.877(2) _cell_angle_alpha 90 _cell_angle_beta 104.490(8) _cell_angle_gamma 90 _cell_volume 2871.3(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.8 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 296.2 #--------------------------------------------------------------------------- #-- _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.400 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.070 _exptl_crystal_F_000 1064.00 _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 0.991 _exptl_special_details ; ? ; #--------------------------------------------------------------------------- #-- _diffrn_special_details ; ? ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 5552 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 0.9986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.9986 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.48 _reflns_number_total 5047 _reflns_number_gt 2461 _reflns_threshold_expression F^2^>2.0\s(F^2^) _diffrn_orient_matrix_UB_11 0.042890 _diffrn_orient_matrix_UB_12 0.001670 _diffrn_orient_matrix_UB_13 0.053550 _diffrn_orient_matrix_UB_21 0.056720 _diffrn_orient_matrix_UB_22 -0.019110 _diffrn_orient_matrix_UB_23 -0.020890 _diffrn_orient_matrix_UB_31 0.012030 _diffrn_orient_matrix_UB_32 0.084170 _diffrn_orient_matrix_UB_33 -0.005800 #--------------------------------------------------------------------------- #-- _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 5047 _refine_ls_number_parameters 407 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.04000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_R_factor_all 0.11702 _refine_ls_R_factor_gt 0.07400 _refine_ls_wR_factor_ref 0.20145 _refine_ls_wR_factor_gt 0.18329 _refine_ls_goodness_of_fit_ref 1.750 _refine_ls_shift/su_max 0.0009 _refine_diff_density_max 0.37 _refine_diff_density_min -0.32 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0027(8) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H H 0.000 0.000 'International Tables Vol C Table 6.1.1.2' N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' #--------------------------------------------------------------------------- #-- 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_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O -0.2304(2) -0.7829(2) -0.5518(1) 0.0670(7) Uani 1.00 d . . . O(2) O -0.3602(1) -0.4721(1) -0.4589(1) 0.0490(6) Uani 1.00 d . . . N(1) N -0.3588(2) -0.6660(2) -0.2181(1) 0.0752(9) Uani 1.00 d . . . C(1) C -0.2656(2) -0.6870(2) -0.5679(2) 0.0456(8) Uani 1.00 d . . . C(2) C -0.2446(2) -0.6141(2) -0.6300(2) 0.0462(8) Uani 1.00 d . . . C(3) C -0.2038(2) -0.6641(3) -0.6851(2) 0.056(1) Uani 1.00 d . . . C(4) C -0.1894(3) -0.6016(3) -0.7455(2) 0.065(1) Uani 1.00 d . . . C(5) C -0.2134(3) -0.4867(3) -0.7517(2) 0.066(1) Uani 1.00 d . . . C(6) C -0.2519(2) -0.4339(3) -0.6967(2) 0.057(1) Uani 1.00 d . . . C(7) C -0.2687(2) -0.4959(2) -0.6353(2) 0.0456(8) Uani 1.00 d . . . C(8) C -0.3053(2) -0.4397(2) -0.5737(2) 0.0437(8) Uani 1.00 d . . . C(9) C -0.3346(2) -0.5094(2) -0.5251(2) 0.0430(7) Uani 1.00 d . . . C(10) C -0.3555(2) -0.5699(2) -0.4121(2) 0.0452(8) Uani 1.00 d . . . C(11) C -0.3642(2) -0.5638(3) -0.3369(2) 0.0528(9) Uani 1.00 d . . . C(12) C -0.3537(2) -0.6665(3) -0.2942(2) 0.0552(9) Uani 1.00 d . . . C(13) C -0.3358(2) -0.7684(3) -0.3303(2) 0.0550(9) Uani 1.00 d . . . C(14) C -0.3279(2) -0.7699(3) -0.4060(2) 0.0515(9) Uani 1.00 d . . . C(15) C -0.3378(2) -0.6694(2) -0.4478(2) 0.0431(7) Uani 1.00 d . . . C(16) C -0.3410(2) -0.6384(2) -0.5309(2) 0.0418(7) Uani 1.00 d . . . C(17) C -0.3052(2) -0.3114(2) -0.5659(1) 0.0458(7) Uani 1.00 d . . . C(18) C -0.3889(3) -0.2524(3) -0.5661(2) 0.060(1) Uani 1.00 d . . . C(19) C -0.3871(4) -0.1337(3) -0.5560(2) 0.079(1) Uani 1.00 d . . . C(20) C -0.3040(4) -0.0735(3) -0.5462(2) 0.076(1) Uani 1.00 d . . . C(21) C -0.2211(3) -0.1297(3) -0.5466(2) 0.071(1) Uani 1.00 d . . . C(22) C -0.2211(3) -0.2485(3) -0.5561(2) 0.0562(9) Uani 1.00 d . . . C(23) C -0.4413(2) -0.6661(3) -0.5867(2) 0.0514(8) Uani 1.00 d . . . C(24) C -0.4680(3) -0.7912(3) -0.6002(2) 0.0628(10) Uani 1.00 d . . . C(25) C -0.5723(3) -0.8044(3) -0.6493(2) 0.086(1) Uani 1.00 d . . . C(26) C -0.6039(3) -0.9253(4) -0.6641(3) 0.115(2) Uani 1.00 d . . . C(27) C -0.3375(3) -0.7684(3) -0.1695(2) 0.072(1) Uani 1.00 d . . . C(28) C -0.4224(3) -0.8440(3) -0.1695(2) 0.083(1) Uani 1.00 d . . . C(29) C -0.3919(3) -0.9528(4) -0.1205(3) 0.112(2) Uani 1.00 d . . . C(30) C -0.4716(4) -1.0263(5) -0.1076(4) 0.202(3) Uani 1.00 d . . . C(31) C -0.3765(4) -0.5597(4) -0.1793(2) 0.111(2) Uani 1.00 d . . . C(32) C -0.4792(4) -0.5251(6) -0.1962(3) 0.157(2) Uani 1.00 d . . . C(33) C -0.5047(7) -0.4013(7) -0.1719(5) 0.235(4) Uani 1.00 d . . . C(34) C -0.4679(7) -0.3880(8) -0.0874(5) 0.262(4) Uani 1.00 d . . . H(1) H -0.184(2) -0.744(2) -0.675(1) 0.058(9) Uiso 1.00 calc . . . H(2) H -0.159(2) -0.642(2) -0.780(2) 0.061(8) Uiso 1.00 calc . . . H(3) H -0.199(3) -0.444(3) -0.787(2) 0.11(1) Uiso 1.00 calc . . . H(4) H -0.266(2) -0.353(2) -0.702(1) 0.052(8) Uiso 1.00 calc . . . H(5) H -0.382(2) -0.498(2) -0.316(1) 0.042(7) Uiso 1.00 calc . . . H(6) H -0.328(2) -0.835(2) -0.304(1) 0.039(7) Uiso 1.00 calc . . . H(7) H -0.315(2) -0.841(2) -0.426(1) 0.046(8) Uiso 1.00 calc . . . H(8) H -0.447(2) -0.295(3) -0.576(2) 0.08(1) Uiso 1.00 calc . . . H(9) H -0.448(3) -0.100(3) -0.564(2) 0.10(1) Uiso 1.00 calc . . . H(10) H -0.304(2) 0.009(3) -0.543(2) 0.09(1) Uiso 1.00 calc . . . H(11) H -0.165(2) -0.093(2) -0.539(2) 0.058(9) Uiso 1.00 calc . . . H(12) H -0.160(2) -0.285(2) -0.553(1) 0.051(8) Uiso 1.00 calc . . . H(13) H -0.447(2) -0.622(3) -0.649(2) 0.092(10) Uiso 1.00 calc . . . H(14) H -0.492(2) -0.640(2) -0.564(1) 0.052(8) Uiso 1.00 calc . . . H(15) H -0.422(2) -0.833(2) -0.626(1) 0.048(8) Uiso 1.00 calc . . . H(16) H -0.459(2) -0.831(3) -0.553(2) 0.08(1) Uiso 1.00 calc . . . H(17) H -0.5783 -0.7653 -0.6966 0.1021 Uiso 1.00 calc . . . H(18) H -0.6143 -0.7670 -0.6217 0.1021 Uiso 1.00 calc . . . H(19) H -0.5606 -0.9639 -0.6880 0.1392 Uiso 1.00 calc . . . H(20) H -0.6671 -0.9271 -0.6974 0.1392 Uiso 1.00 calc . . . H(21) H -0.6040 -0.9625 -0.6168 0.1392 Uiso 1.00 calc . . . H(22) H -0.287(2) -0.818(3) -0.193(2) 0.09(1) Uiso 1.00 calc . . . H(23) H -0.306(3) -0.735(3) -0.118(2) 0.11(1) Uiso 1.00 calc . . . H(24) H -0.4517 -0.8663 -0.2209 0.0994 Uiso 1.00 calc . . . H(25) H -0.4671 -0.8019 -0.1488 0.0994 Uiso 1.00 calc . . . H(26) H -0.3542 -0.9991 -0.1453 0.1303 Uiso 1.00 calc . . . H(27) H -0.3544 -0.9297 -0.0712 0.1303 Uiso 1.00 calc . . . H(28) H -0.5069 -1.0516 -0.1560 0.2479 Uiso 1.00 calc . . . H(29) H -0.4424 -1.0888 -0.0764 0.2479 Uiso 1.00 calc . . . H(30) H -0.5082 -0.9811 -0.0825 0.2479 Uiso 1.00 calc . . . H(31) H -0.3411 -0.4989 -0.1953 0.1345 Uiso 1.00 calc . . . H(32) H -0.3535 -0.5705 -0.1251 0.1345 Uiso 1.00 calc . . . H(33) H -0.5045 -0.5302 -0.2505 0.1894 Uiso 1.00 calc . . . H(34) H -0.5112 -0.5793 -0.1713 0.1894 Uiso 1.00 calc . . . H(35) H -0.4754 -0.3454 -0.1969 0.2802 Uiso 1.00 calc . . . H(36) H -0.5718 -0.3918 -0.1839 0.2802 Uiso 1.00 calc . . . H(37) H -0.4011 -0.4021 -0.0771 0.3066 Uiso 1.00 calc . . . H(38) H -0.5004 -0.4386 -0.0647 0.3066 Uiso 1.00 calc . . . H(39) H -0.4797 -0.3097 -0.0777 0.3066 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) 0.083(2) 0.047(1) 0.081(2) 0.020(1) 0.039(1) 0.012(1) O(2) 0.068(1) 0.039(1) 0.047(1) 0.0035(10) 0.027(1) 0.0012(8) N(1) 0.115(2) 0.069(2) 0.048(1) -0.006(2) 0.034(2) 0.006(1) C(1) 0.050(2) 0.041(1) 0.045(2) 0.002(1) 0.011(1) -0.002(1) C(2) 0.051(2) 0.045(1) 0.044(2) -0.001(1) 0.015(1) -0.005(1) C(3) 0.065(2) 0.056(2) 0.051(2) 0.000(2) 0.023(2) -0.011(1) C(4) 0.083(3) 0.072(2) 0.049(2) 0.003(2) 0.033(2) -0.009(2) C(5) 0.088(3) 0.066(2) 0.049(2) -0.004(2) 0.029(2) 0.000(2) C(6) 0.081(2) 0.053(2) 0.041(2) 0.000(2) 0.020(2) 0.005(1) C(7) 0.050(2) 0.047(1) 0.041(1) -0.003(1) 0.015(1) -0.003(1) C(8) 0.050(2) 0.043(1) 0.039(1) -0.002(1) 0.014(1) -0.002(1) C(9) 0.052(2) 0.039(1) 0.040(1) 0.005(1) 0.016(1) -0.002(1) C(10) 0.052(2) 0.039(1) 0.046(1) 0.000(1) 0.017(1) 0.004(1) C(11) 0.069(2) 0.047(2) 0.046(2) 0.003(2) 0.023(2) -0.005(1) C(12) 0.070(2) 0.054(2) 0.044(1) -0.002(2) 0.018(2) 0.003(1) C(13) 0.071(2) 0.046(2) 0.049(2) 0.001(2) 0.016(2) 0.014(1) C(14) 0.067(2) 0.040(2) 0.049(2) 0.003(2) 0.019(2) 0.004(1) C(15) 0.050(2) 0.040(1) 0.040(1) 0.000(1) 0.013(1) 0.000(1) C(16) 0.050(1) 0.036(1) 0.041(1) 0.002(1) 0.014(1) -0.001(1) C(17) 0.065(2) 0.040(1) 0.036(2) 0.001(1) 0.020(1) 0.003(1) C(18) 0.073(2) 0.048(2) 0.067(2) 0.007(2) 0.030(2) 0.008(2) C(19) 0.117(3) 0.050(2) 0.083(3) 0.026(2) 0.047(3) 0.013(2) C(20) 0.135(3) 0.043(2) 0.059(2) 0.003(2) 0.043(2) 0.001(2) C(21) 0.103(3) 0.058(2) 0.052(2) -0.031(2) 0.021(2) -0.005(2) C(22) 0.067(2) 0.054(2) 0.049(2) -0.005(2) 0.017(2) 0.002(2) C(23) 0.048(2) 0.053(2) 0.052(2) 0.002(1) 0.011(1) -0.001(1) C(24) 0.065(2) 0.057(2) 0.066(2) -0.008(2) 0.015(2) -0.007(2) C(25) 0.067(2) 0.078(2) 0.104(3) -0.019(2) 0.006(2) -0.011(2) C(26) 0.105(3) 0.086(2) 0.136(4) -0.023(3) -0.005(3) -0.024(3) C(27) 0.094(3) 0.075(2) 0.045(2) -0.009(2) 0.016(2) 0.009(2) C(28) 0.084(2) 0.087(3) 0.081(3) 0.001(2) 0.028(2) 0.017(2) C(29) 0.118(3) 0.087(3) 0.116(4) 0.005(2) 0.003(3) 0.030(2) C(30) 0.130(5) 0.191(6) 0.266(8) -0.044(4) 0.013(5) 0.147(6) C(31) 0.181(4) 0.103(3) 0.063(3) 0.033(3) 0.055(3) 0.012(2) C(32) 0.173(4) 0.187(5) 0.119(4) 0.048(5) 0.051(4) 0.049(4) C(33) 0.32(1) 0.194(7) 0.232(7) 0.020(8) 0.140(8) -0.048(7) C(34) 0.239(9) 0.259(9) 0.265(8) -0.009(7) 0.019(8) -0.111(9) #--------------------------------------------------------------------------- #-- _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) 1.224(4) . . yes O(2) C(9) 1.393(4) . . yes O(2) C(10) 1.399(4) . . yes N(1) C(12) 1.380(5) . . yes N(1) C(27) 1.456(5) . . yes N(1) C(31) 1.465(6) . . yes C(1) C(2) 1.485(5) . . yes C(1) C(16) 1.510(5) . . yes C(2) C(3) 1.391(5) . . yes C(2) C(7) 1.410(5) . . yes C(3) C(4) 1.359(6) . . yes C(4) C(5) 1.373(6) . . yes C(5) C(6) 1.384(6) . . yes C(6) C(7) 1.383(5) . . yes C(7) C(8) 1.482(5) . . yes C(8) C(9) 1.329(5) . . yes C(8) C(17) 1.492(5) . . yes C(9) C(16) 1.499(5) . . yes C(10) C(11) 1.383(5) . . yes C(10) C(15) 1.372(5) . . yes C(11) C(12) 1.401(5) . . yes C(12) C(13) 1.400(5) . . yes C(13) C(14) 1.385(5) . . yes C(14) C(15) 1.372(5) . . yes C(15) C(16) 1.517(5) . . yes C(16) C(23) 1.563(5) . . yes C(17) C(18) 1.380(5) . . yes C(17) C(22) 1.381(5) . . yes C(18) C(19) 1.386(6) . . yes C(19) C(20) 1.352(7) . . yes C(20) C(21) 1.356(7) . . yes C(21) C(22) 1.386(6) . . yes C(23) C(24) 1.503(6) . . yes C(24) C(25) 1.539(6) . . yes C(25) C(26) 1.475(7) . . yes C(27) C(28) 1.498(7) . . yes C(28) C(29) 1.534(7) . . yes C(29) C(30) 1.487(7) . . yes C(31) C(32) 1.482(7) . . yes C(32) C(33) 1.568(8) . . yes C(33) C(34) 1.478(9) . . 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(9) O(2) C(10) 105.9(3) . . . yes C(12) N(1) C(27) 122.0(4) . . . yes C(12) N(1) C(31) 121.8(4) . . . yes C(27) N(1) C(31) 115.9(4) . . . yes O(1) C(1) C(2) 122.9(3) . . . yes O(1) C(1) C(16) 122.3(3) . . . yes C(2) C(1) C(16) 114.6(3) . . . yes C(1) C(2) C(3) 119.5(4) . . . yes C(1) C(2) C(7) 120.7(3) . . . yes C(3) C(2) C(7) 119.8(4) . . . yes C(2) C(3) C(4) 121.0(4) . . . yes C(3) C(4) C(5) 119.8(4) . . . yes C(4) C(5) C(6) 120.5(4) . . . yes C(5) C(6) C(7) 121.0(4) . . . yes C(2) C(7) C(6) 118.0(4) . . . yes C(2) C(7) C(8) 120.2(3) . . . yes C(6) C(7) C(8) 121.7(4) . . . yes C(7) C(8) C(9) 116.5(3) . . . yes C(7) C(8) C(17) 121.0(3) . . . yes C(9) C(8) C(17) 122.5(3) . . . yes O(2) C(9) C(8) 124.1(3) . . . yes O(2) C(9) C(16) 110.0(3) . . . yes C(8) C(9) C(16) 125.8(3) . . . yes O(2) C(10) C(11) 122.5(3) . . . yes O(2) C(10) C(15) 112.9(3) . . . yes C(11) C(10) C(15) 124.5(4) . . . yes C(10) C(11) C(12) 117.7(4) . . . yes N(1) C(12) C(11) 120.6(4) . . . yes N(1) C(12) C(13) 121.3(4) . . . yes C(11) C(12) C(13) 118.1(4) . . . yes C(12) C(13) C(14) 122.0(4) . . . yes C(13) C(14) C(15) 120.0(4) . . . yes C(10) C(15) C(14) 117.7(3) . . . yes C(10) C(15) C(16) 107.0(3) . . . yes C(14) C(15) C(16) 135.1(3) . . . yes C(1) C(16) C(9) 111.3(3) . . . yes C(1) C(16) C(15) 119.4(3) . . . yes C(1) C(16) C(23) 106.7(3) . . . yes C(9) C(16) C(15) 100.5(3) . . . yes C(9) C(16) C(23) 106.2(3) . . . yes C(15) C(16) C(23) 112.0(3) . . . yes C(8) C(17) C(18) 120.8(4) . . . yes C(8) C(17) C(22) 121.2(4) . . . yes C(18) C(17) C(22) 118.0(4) . . . yes C(17) C(18) C(19) 120.2(5) . . . yes C(18) C(19) C(20) 121.0(5) . . . yes C(19) C(20) C(21) 119.7(5) . . . yes C(20) C(21) C(22) 120.2(5) . . . yes C(17) C(22) C(21) 120.9(5) . . . yes C(16) C(23) C(24) 117.2(4) . . . yes C(23) C(24) C(25) 111.0(4) . . . yes C(24) C(25) C(26) 114.0(4) . . . yes N(1) C(27) C(28) 115.3(4) . . . yes C(27) C(28) C(29) 111.5(4) . . . yes C(28) C(29) C(30) 116.1(5) . . . yes N(1) C(31) C(32) 114.3(6) . . . yes C(31) C(32) C(33) 118.6(8) . . . yes C(32) C(33) C(34) 109.3(10) . . . yes #--------------------------------------------------------------------------- #-- #===============================================END data_2b _database_code_depnum_ccdc_archive 'CCDC 605726' _audit_creation_date 'Wed Jan 4 21:54:43 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #--------------------------------------------------------------------------- #-- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------------- #-- _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 513.68 _chemical_formula_analytical ? _chemical_formula_sum ' C36 H35 N O2 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_melting_point ? #--------------------------------------------------------------------------- #-- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 9.081(2) _cell_length_b 20.626(4) _cell_length_c 15.600(3) _cell_angle_alpha 90 _cell_angle_beta 98.69(2) _cell_angle_gamma 90 _cell_volume 2888(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.1 _cell_measurement_theta_max 12.7 _cell_measurement_temperature 296.2 #--------------------------------------------------------------------------- #-- _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.072 _exptl_crystal_F_000 1096.00 _exptl_absorpt_correction_T_min 0.956 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #--------------------------------------------------------------------------- #-- _diffrn_special_details ; ? ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 5427 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 0.9988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.9988 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.31 _reflns_number_total 5087 _reflns_number_gt 1900 _reflns_threshold_expression F^2^>2.0\s(F^2^) _diffrn_orient_matrix_UB_11 0.011690 _diffrn_orient_matrix_UB_12 0.036230 _diffrn_orient_matrix_UB_13 0.043090 _diffrn_orient_matrix_UB_21 0.007260 _diffrn_orient_matrix_UB_22 0.031670 _diffrn_orient_matrix_UB_23 -0.047710 _diffrn_orient_matrix_UB_31 -0.110540 _diffrn_orient_matrix_UB_32 0.005910 _diffrn_orient_matrix_UB_33 -0.008450 #--------------------------------------------------------------------------- _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 5087 _refine_ls_number_parameters 457 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.04000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_R_factor_all 0.15362 _refine_ls_R_factor_gt 0.06905 _refine_ls_wR_factor_ref 0.20345 _refine_ls_wR_factor_gt 0.15930 _refine_ls_goodness_of_fit_ref 1.423 _refine_ls_shift/su_max 0.0029 _refine_diff_density_max 0.44 _refine_diff_density_min -0.37 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0035(9) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H H 0.000 0.000 'International Tables Vol C Table 6.1.1.2' N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' #--------------------------------------------------------------------------- #-- 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_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.4279(3) 0.0760(1) 0.1114(2) 0.079(1) Uani 1.00 d . . . O(2) O 0.4864(3) 0.2736(1) -0.0085(2) 0.0583(9) Uani 1.00 d . . . N(1) N 0.1447(4) 0.2282(2) -0.2702(2) 0.076(1) Uani 1.00 d . . . C(1) C 0.5029(5) 0.1249(2) 0.1181(3) 0.057(1) Uani 1.00 d . . . C(2) C 0.5866(5) 0.1479(2) 0.2019(3) 0.058(1) Uani 1.00 d . . . C(3) C 0.6192(6) 0.1039(3) 0.2691(3) 0.076(2) Uani 1.00 d . . . C(4) C 0.7016(7) 0.1222(3) 0.3471(3) 0.094(2) Uani 1.00 d . . . C(5) C 0.7530(7) 0.1858(3) 0.3578(3) 0.084(2) Uani 1.00 d . . . C(6) C 0.7196(5) 0.2301(2) 0.2906(3) 0.063(1) Uani 1.00 d . . . C(7) C 0.6359(4) 0.2132(2) 0.2112(3) 0.053(1) Uani 1.00 d . . . C(8) C 0.5942(4) 0.2604(2) 0.1406(3) 0.049(1) Uani 1.00 d . . . C(9) C 0.5428(4) 0.2359(2) 0.0631(3) 0.048(1) Uani 1.00 d . . . C(10) C 0.3973(4) 0.2317(2) -0.0656(3) 0.053(1) Uani 1.00 d . . . C(11) C 0.3146(5) 0.2543(2) -0.1410(3) 0.058(1) Uani 1.00 d . . . C(12) C 0.2278(4) 0.2090(2) -0.1927(3) 0.060(1) Uani 1.00 d . . . C(13) C 0.2286(5) 0.1439(2) -0.1638(3) 0.065(1) Uani 1.00 d . . . C(14) C 0.3176(5) 0.1240(2) -0.0889(3) 0.059(1) Uani 1.00 d . . . C(15) C 0.4052(4) 0.1685(2) -0.0374(3) 0.051(1) Uani 1.00 d . . . C(16) C 0.5272(4) 0.1650(2) 0.0400(3) 0.047(1) Uani 1.00 d . . . C(17) C 0.6044(4) 0.3312(2) 0.1557(3) 0.054(1) Uani 1.00 d . . . C(18) C 0.6612(5) 0.3709(2) 0.0968(3) 0.066(1) Uani 1.00 d . . . C(19) C 0.6691(6) 0.4378(3) 0.1071(4) 0.085(2) Uani 1.00 d . . . C(20) C 0.6215(6) 0.4662(3) 0.1796(4) 0.088(2) Uani 1.00 d . . . C(21) C 0.5645(6) 0.4270(3) 0.2381(4) 0.085(2) Uani 1.00 d . . . C(22) C 0.5568(5) 0.3605(2) 0.2272(3) 0.064(1) Uani 1.00 d . . . C(23) C 0.6713(4) 0.1378(2) 0.0113(2) 0.045(1) Uani 1.00 d . . . C(24) C 0.7941(5) 0.1753(2) 0.0058(3) 0.057(1) Uani 1.00 d . . . C(25) C 0.9189(5) 0.1511(3) -0.0263(3) 0.071(2) Uani 1.00 d . . . C(26) C 0.9190(5) 0.0873(3) -0.0498(3) 0.071(1) Uani 1.00 d . . . C(27) C 0.7993(5) 0.0479(2) -0.0434(3) 0.073(2) Uani 1.00 d . . . C(28) C 0.6752(5) 0.0731(2) -0.0129(3) 0.061(1) Uani 1.00 d . . . C(29) C 0.0429(6) 0.1836(3) -0.3212(4) 0.105(2) Uani 1.00 d . . . C(30) C 0.105(1) 0.1342(4) -0.3732(6) 0.223(5) Uani 1.00 d . . . C(31) C 0.158(1) 0.1491(5) -0.4558(7) 0.285(7) Uani 1.00 d . . . C(32) C 0.206(1) 0.0904(5) -0.4992(5) 0.212(5) Uani 1.00 d . . . C(33) C 0.1595(6) 0.2928(3) -0.3044(3) 0.077(2) Uani 1.00 d . . . C(34) C 0.0598(6) 0.3430(3) -0.2715(4) 0.079(2) Uani 1.00 d . . . C(35) C 0.0913(7) 0.4115(3) -0.3001(4) 0.096(2) Uani 1.00 d . . . C(36) C -0.006(1) 0.4633(4) -0.2710(6) 0.122(3) Uani 1.00 d . . . H(1) H 0.587(6) 0.061(3) 0.259(3) 0.14(2) Uiso 1.00 calc . . . H(2) H 0.747(6) 0.089(3) 0.397(3) 0.14(1) Uiso 1.00 calc . . . H(3) H 0.819(4) 0.200(2) 0.416(2) 0.06(1) Uiso 1.00 calc . . . H(4) H 0.762(4) 0.276(2) 0.294(2) 0.050(10) Uiso 1.00 calc . . . H(5) H 0.321(4) 0.299(2) -0.156(2) 0.07(1) Uiso 1.00 calc . . . H(6) H 0.168(4) 0.112(2) -0.207(2) 0.05(1) Uiso 1.00 calc . . . H(7) H 0.318(5) 0.075(2) -0.060(3) 0.10(1) Uiso 1.00 calc . . . H(8) H 0.695(4) 0.351(2) 0.045(3) 0.07(1) Uiso 1.00 calc . . . H(9) H 0.709(6) 0.464(3) 0.061(3) 0.14(1) Uiso 1.00 calc . . . H(10) H 0.614(5) 0.523(2) 0.190(3) 0.13(1) Uiso 1.00 calc . . . H(11) H 0.539(4) 0.447(2) 0.290(3) 0.08(1) Uiso 1.00 calc . . . H(12) H 0.516(4) 0.331(2) 0.277(3) 0.09(1) Uiso 1.00 calc . . . H(13) H 0.794(4) 0.215(2) 0.026(2) 0.06(1) Uiso 1.00 calc . . . H(14) H 1.008(5) 0.178(2) -0.038(3) 0.11(1) Uiso 1.00 calc . . . H(15) H 1.014(5) 0.068(2) -0.072(3) 0.10(1) Uiso 1.00 calc . . . H(16) H 0.797(6) -0.002(3) -0.054(4) 0.17(2) Uiso 1.00 calc . . . H(17) H 0.589(5) 0.042(2) -0.011(3) 0.10(1) Uiso 1.00 calc . . . H(27) H 0.141(5) 0.294(3) -0.377(3) 0.14(1) Uiso 1.00 calc . . . H(28) H 0.272(6) 0.304(2) -0.290(3) 0.12(1) Uiso 1.00 calc . . . H(29) H 0.078(5) 0.349(2) -0.211(3) 0.10(1) Uiso 1.00 calc . . . H(30) H -0.052(5) 0.329(2) -0.300(3) 0.08(1) Uiso 1.00 calc . . . H(31) H 0.100(7) 0.403(4) -0.380(5) 0.23(2) Uiso 1.00 calc . . . H(32) H 0.185(6) 0.424(3) -0.278(4) 0.14(2) Uiso 1.00 calc . . . H(33) H 0.002(8) 0.456(4) -0.210(4) 0.17(2) Uiso 1.00 calc . . . H(34) H -0.099(10) 0.451(5) -0.306(6) 0.26(3) Uiso 1.00 calc . . . H(35) H 0.01(1) 0.505(5) -0.276(8) 0.36(5) Uiso 1.00 calc . . . H(36) H 0.1903 0.1175 -0.3372 0.2560 Uiso 1.00 calc . . . H(37) H 0.0322 0.1021 -0.3858 0.2560 Uiso 1.00 calc . . . H(38) H 0.0755 0.1679 -0.4923 0.3397 Uiso 1.00 calc . . . H(39) H 0.2363 0.1783 -0.4444 0.3397 Uiso 1.00 calc . . . H(40) H 0.1266 0.0607 -0.5117 0.2516 Uiso 1.00 calc . . . H(41) H 0.2386 0.1037 -0.5520 0.2516 Uiso 1.00 calc . . . H(42) H 0.2870 0.0706 -0.4629 0.2516 Uiso 1.00 calc . . . H(43) H -0.0108 0.1620 -0.2816 0.1266 Uiso 1.00 calc . . . H(44) H -0.0257 0.2099 -0.3590 0.1266 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) 0.093(3) 0.064(2) 0.085(2) -0.032(2) 0.028(2) -0.001(2) O(2) 0.066(2) 0.048(2) 0.056(2) -0.004(1) -0.005(1) -0.002(1) N(1) 0.064(2) 0.093(3) 0.067(2) -0.007(2) -0.009(2) 0.001(2) C(1) 0.063(3) 0.049(2) 0.063(2) 0.002(2) 0.026(2) -0.003(2) C(2) 0.066(3) 0.055(2) 0.057(2) 0.001(2) 0.025(2) -0.001(2) C(3) 0.104(4) 0.062(3) 0.068(3) 0.005(3) 0.035(3) 0.012(2) C(4) 0.148(6) 0.079(3) 0.059(3) 0.013(3) 0.029(3) 0.014(3) C(5) 0.116(5) 0.082(3) 0.054(3) 0.018(3) 0.013(3) 0.005(2) C(6) 0.076(3) 0.062(3) 0.053(2) 0.003(3) 0.014(2) -0.010(2) C(7) 0.054(3) 0.054(2) 0.053(2) 0.008(2) 0.017(2) 0.000(2) C(8) 0.049(2) 0.051(2) 0.050(2) -0.001(2) 0.012(2) -0.004(2) C(9) 0.050(2) 0.044(2) 0.051(2) -0.001(2) 0.009(2) -0.001(2) C(10) 0.047(2) 0.050(2) 0.061(2) -0.001(2) 0.006(2) -0.013(2) C(11) 0.054(3) 0.054(3) 0.065(3) 0.002(2) 0.006(2) -0.001(2) C(12) 0.044(2) 0.074(2) 0.062(3) 0.001(2) 0.004(2) -0.006(2) C(13) 0.052(3) 0.068(3) 0.073(3) -0.015(2) 0.000(2) -0.011(2) C(14) 0.052(3) 0.057(3) 0.068(3) -0.011(2) 0.011(2) -0.013(2) C(15) 0.047(2) 0.052(2) 0.056(2) 0.000(2) 0.010(2) -0.007(2) C(16) 0.048(2) 0.042(2) 0.052(2) -0.005(2) 0.011(2) -0.004(2) C(17) 0.050(2) 0.053(2) 0.060(3) -0.003(2) 0.007(2) -0.010(2) C(18) 0.075(3) 0.059(2) 0.067(3) -0.011(2) 0.021(3) -0.006(2) C(19) 0.091(4) 0.060(2) 0.108(4) -0.021(3) 0.031(3) -0.008(3) C(20) 0.096(4) 0.054(3) 0.117(4) -0.012(3) 0.028(3) -0.025(3) C(21) 0.106(4) 0.066(2) 0.087(4) -0.001(3) 0.023(3) -0.033(3) C(22) 0.071(3) 0.061(2) 0.065(3) 0.002(2) 0.022(2) -0.013(2) C(23) 0.047(2) 0.045(2) 0.043(2) 0.000(2) 0.003(2) -0.003(2) C(24) 0.059(2) 0.049(3) 0.067(3) -0.012(2) 0.017(2) -0.014(2) C(25) 0.055(3) 0.077(3) 0.084(4) -0.005(3) 0.020(2) -0.006(3) C(26) 0.055(3) 0.080(3) 0.080(3) 0.008(2) 0.018(3) -0.008(3) C(27) 0.066(3) 0.060(3) 0.095(4) 0.002(2) 0.018(3) -0.023(3) C(28) 0.064(3) 0.044(2) 0.078(3) -0.004(2) 0.019(2) -0.008(2) C(29) 0.079(4) 0.113(5) 0.106(5) -0.021(3) -0.041(3) -0.009(3) C(30) 0.220(10) 0.25(1) 0.179(8) 0.122(8) -0.026(7) -0.142(7) C(31) 0.40(2) 0.26(1) 0.21(1) 0.19(1) 0.10(1) -0.038(9) C(32) 0.27(1) 0.217(10) 0.141(8) 0.060(8) 0.020(7) -0.045(7) C(33) 0.070(3) 0.102(3) 0.058(3) -0.004(3) 0.003(3) 0.007(3) C(34) 0.067(3) 0.096(3) 0.071(4) -0.005(3) 0.002(3) 0.007(3) C(35) 0.101(5) 0.092(3) 0.096(5) -0.023(3) 0.018(4) -0.005(4) C(36) 0.126(6) 0.096(6) 0.152(8) 0.016(5) 0.042(6) 0.012(6) #--------------------------------------------------------------------------- #-- _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) 1.213(5) . . yes O(2) C(9) 1.394(5) . . yes O(2) C(10) 1.406(5) . . yes N(1) C(12) 1.383(6) . . yes N(1) C(29) 1.454(7) . . yes N(1) C(33) 1.449(7) . . yes C(1) C(2) 1.487(7) . . yes C(1) C(16) 1.518(6) . . yes C(2) C(3) 1.383(7) . . yes C(2) C(7) 1.420(6) . . yes C(3) C(4) 1.381(9) . . yes C(4) C(5) 1.395(9) . . yes C(5) C(6) 1.388(8) . . yes C(6) C(7) 1.396(7) . . yes C(7) C(8) 1.477(6) . . yes C(8) C(9) 1.327(6) . . yes C(8) C(17) 1.481(6) . . yes C(9) C(16) 1.507(6) . . yes C(10) C(11) 1.377(7) . . yes C(10) C(15) 1.375(6) . . yes C(11) C(12) 1.398(7) . . yes C(12) C(13) 1.415(7) . . yes C(13) C(14) 1.379(7) . . yes C(14) C(15) 1.387(6) . . yes C(15) C(16) 1.512(6) . . yes C(16) C(23) 1.551(6) . . yes C(17) C(18) 1.387(7) . . yes C(17) C(22) 1.393(6) . . yes C(18) C(19) 1.389(8) . . yes C(19) C(20) 1.398(8) . . yes C(20) C(21) 1.379(8) . . yes C(21) C(22) 1.381(8) . . yes C(23) C(24) 1.370(6) . . yes C(23) C(28) 1.390(6) . . yes C(24) C(25) 1.400(7) . . yes C(25) C(26) 1.366(8) . . yes C(26) C(27) 1.373(8) . . yes C(27) C(28) 1.389(7) . . yes C(29) C(30) 1.466(10) . . yes C(30) C(31) 1.477(9) . . yes C(31) C(32) 1.48(1) . . yes C(33) C(34) 1.516(8) . . yes C(34) C(35) 1.521(9) . . yes C(35) C(36) 1.50(1) . . 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(9) O(2) C(10) 105.8(4) . . . yes C(12) N(1) C(29) 121.0(5) . . . yes C(12) N(1) C(33) 121.1(5) . . . yes C(29) N(1) C(33) 117.8(5) . . . yes O(1) C(1) C(2) 123.2(5) . . . yes O(1) C(1) C(16) 122.1(5) . . . yes C(2) C(1) C(16) 114.6(4) . . . yes C(1) C(2) C(3) 118.6(5) . . . yes C(1) C(2) C(7) 120.2(5) . . . yes C(3) C(2) C(7) 121.1(5) . . . yes C(2) C(3) C(4) 120.9(6) . . . yes C(3) C(4) C(5) 119.3(6) . . . yes C(4) C(5) C(6) 119.9(6) . . . yes C(5) C(6) C(7) 122.2(6) . . . yes C(2) C(7) C(6) 116.6(5) . . . yes C(2) C(7) C(8) 120.5(4) . . . yes C(6) C(7) C(8) 122.8(5) . . . yes C(7) C(8) C(9) 116.3(4) . . . yes C(7) C(8) C(17) 121.9(4) . . . yes C(9) C(8) C(17) 121.8(5) . . . yes O(2) C(9) C(8) 123.6(4) . . . yes O(2) C(9) C(16) 109.8(4) . . . yes C(8) C(9) C(16) 126.5(4) . . . yes O(2) C(10) C(11) 121.4(5) . . . yes O(2) C(10) C(15) 112.5(4) . . . yes C(11) C(10) C(15) 126.1(5) . . . yes C(10) C(11) C(12) 117.0(5) . . . yes N(1) C(12) C(11) 119.9(5) . . . yes N(1) C(12) C(13) 121.8(5) . . . yes C(11) C(12) C(13) 118.3(5) . . . yes C(12) C(13) C(14) 121.7(5) . . . yes C(13) C(14) C(15) 120.4(5) . . . yes C(10) C(15) C(14) 116.3(5) . . . yes C(10) C(15) C(16) 107.3(4) . . . yes C(14) C(15) C(16) 135.9(5) . . . yes C(1) C(16) C(9) 110.9(4) . . . yes C(1) C(16) C(15) 119.3(4) . . . yes C(1) C(16) C(23) 105.4(4) . . . yes C(9) C(16) C(15) 100.2(4) . . . yes C(9) C(16) C(23) 111.6(4) . . . yes C(15) C(16) C(23) 109.6(4) . . . yes C(8) C(17) C(18) 119.8(5) . . . yes C(8) C(17) C(22) 122.4(5) . . . yes C(18) C(17) C(22) 117.8(5) . . . yes C(17) C(18) C(19) 121.8(6) . . . yes C(18) C(19) C(20) 119.5(6) . . . yes C(19) C(20) C(21) 118.8(6) . . . yes C(20) C(21) C(22) 121.2(6) . . . yes C(17) C(22) C(21) 120.8(6) . . . yes C(16) C(23) C(24) 122.9(4) . . . yes C(16) C(23) C(28) 118.9(4) . . . yes C(24) C(23) C(28) 118.1(5) . . . yes C(23) C(24) C(25) 122.2(5) . . . yes C(24) C(25) C(26) 118.2(6) . . . yes C(25) C(26) C(27) 121.2(6) . . . yes C(26) C(27) C(28) 119.7(6) . . . yes C(23) C(28) C(27) 120.5(5) . . . yes N(1) C(29) C(30) 118.6(7) . . . yes C(29) C(30) C(31) 122(1) . . . yes C(30) C(31) C(32) 112(1) . . . yes N(1) C(33) C(34) 114.2(5) . . . yes C(33) C(34) C(35) 112.7(6) . . . yes C(34) C(35) C(36) 115.2(7) . . . yes #--------------------------------------------------------------------------- #-- #===============================================END data_2c _database_code_depnum_ccdc_archive 'CCDC 605727' _audit_creation_date 'Thu Jan 5 05:17:39 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #--------------------------------------------------------------------------- #-- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------------- #-- _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 519.70 _chemical_formula_analytical ? _chemical_formula_sum ' C34 H33 N O2 S ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_melting_point ? #--------------------------------------------------------------------------- #-- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.088(8) _cell_length_b 16.317(6) _cell_length_c 9.031(6) _cell_angle_alpha 91.18(4) _cell_angle_beta 97.28(6) _cell_angle_gamma 72.73(4) _cell_volume 1407(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7 _cell_measurement_theta_min 11.2 _cell_measurement_theta_max 12.2 _cell_measurement_temperature 296.2 #--------------------------------------------------------------------------- #-- _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.146 _exptl_crystal_F_000 552.00 _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #--------------------------------------------------------------------------- #-- _diffrn_special_details ; ? ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 6872 _diffrn_reflns_av_R_equivalents 0.084 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0000 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.27 _reflns_number_total 6463 _reflns_number_gt 1656 _reflns_threshold_expression F^2^>2.0\s(F^2^) _diffrn_orient_matrix_UB_11 -0.086450 _diffrn_orient_matrix_UB_12 0.040430 _diffrn_orient_matrix_UB_13 -0.054370 _diffrn_orient_matrix_UB_21 0.015490 _diffrn_orient_matrix_UB_22 0.048050 _diffrn_orient_matrix_UB_23 0.063560 _diffrn_orient_matrix_UB_31 0.056900 _diffrn_orient_matrix_UB_32 0.013320 _diffrn_orient_matrix_UB_33 -0.073960 #--------------------------------------------------------------------------- #-- _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 6463 _refine_ls_number_parameters 392 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.04000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_R_factor_all 0.27713 _refine_ls_R_factor_gt 0.10888 _refine_ls_wR_factor_ref 0.28412 _refine_ls_wR_factor_gt 0.24298 _refine_ls_goodness_of_fit_ref 1.601 _refine_ls_shift/su_max 3.6694 _refine_diff_density_max 1.20 _refine_diff_density_min -1.21 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H H 0.000 0.000 'International Tables Vol C Table 6.1.1.2' N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' S S 0.125 0.123 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' #--------------------------------------------------------------------------- #-- 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_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S(1) S 0.6551(2) 0.1821(2) 0.3721(2) 0.1035(8) Uani 1.00 d . . . O(1) O 0.7211(4) -0.0076(3) -0.0020(5) 0.072(2) Uani 1.00 d . . . O(2) O 0.6546(4) 0.2779(2) -0.0092(4) 0.052(1) Uani 1.00 d . . . N(1) N 0.2487(6) 0.3319(4) -0.3814(6) 0.087(2) Uani 1.00 d . . . C(1) C 0.7557(6) 0.0514(4) 0.0615(6) 0.052(2) Uani 1.00 d . . . C(2) C 0.8960(6) 0.0345(4) 0.1556(6) 0.051(2) Uani 1.00 d . . . C(3) C 0.9659(7) -0.0460(4) 0.2093(8) 0.071(2) Uani 1.00 d . . . C(4) C 1.0913(8) -0.0599(5) 0.3057(9) 0.091(3) Uani 1.00 d . . . C(5) C 1.1388(7) 0.0093(5) 0.3457(9) 0.083(2) Uani 1.00 d . . . C(6) C 1.0679(6) 0.0909(4) 0.2901(7) 0.064(2) Uani 1.00 d . . . C(7) C 0.9442(6) 0.1054(4) 0.1954(6) 0.050(2) Uani 1.00 d . . . C(8) C 0.8683(5) 0.1932(4) 0.1245(6) 0.044(1) Uani 1.00 d . . . C(9) C 0.7374(5) 0.2043(3) 0.0704(6) 0.045(2) Uani 1.00 d . . . C(10) C 0.5439(6) 0.2553(4) -0.0929(6) 0.050(2) Uani 1.00 d . . . C(11) C 0.4513(6) 0.3099(4) -0.1964(6) 0.055(2) Uani 1.00 d . . . C(12) C 0.3432(6) 0.2823(5) -0.2712(6) 0.064(2) Uani 1.00 d . . . C(13) C 0.3389(6) 0.1964(5) -0.2365(7) 0.065(2) Uani 1.00 d . . . C(14) C 0.4397(6) 0.1448(4) -0.1273(7) 0.055(2) Uani 1.00 d . . . C(15) C 0.5432(6) 0.1737(4) -0.0568(6) 0.052(2) Uani 1.00 d . . . C(16) C 0.6573(5) 0.1394(4) 0.0693(6) 0.046(1) Uani 1.00 d . . . C(17) C 0.9400(6) 0.2600(4) 0.1159(6) 0.045(1) Uani 1.00 d . . . C(18) C 0.8744(7) 0.3444(4) 0.1425(7) 0.059(2) Uani 1.00 d . . . C(19) C 0.9371(8) 0.4082(5) 0.1304(7) 0.073(2) Uani 1.00 d . . . C(20) C 1.0708(8) 0.3863(5) 0.0902(7) 0.076(2) Uani 1.00 d . . . C(21) C 1.1401(7) 0.3010(5) 0.0648(7) 0.066(2) Uani 1.00 d . . . C(22) C 1.0757(7) 0.2388(4) 0.0804(6) 0.055(2) Uani 1.00 d . . . C(23) C 0.5956(5) 0.1383(3) 0.2171(6) 0.051(2) Uani 1.00 d . . . C(24) C 0.4838(4) 0.0971(3) 0.2454(5) 0.027(1) Uani 1.00 d . . . C(25) C 0.4754(7) 0.1138(5) 0.4035(7) 0.079(2) Uani 1.00 d . . . C(26) C 0.5523(7) 0.1532(5) 0.4798(7) 0.083(3) Uani 1.00 d . . . C(27) C 0.1372(8) 0.2999(8) -0.4635(9) 0.108(4) Uani 1.00 d . . . C(28) C 0.0141(8) 0.3240(7) -0.3568(9) 0.160(4) Uani 1.00 d . . . C(29) C -0.1083(9) 0.3014(8) -0.4208(10) 0.165(5) Uani 1.00 d . . . C(30) C -0.2130(8) 0.3132(6) -0.3151(10) 0.123(4) Uani 1.00 d . . . C(31) C 0.2538(7) 0.4158(5) -0.4240(9) 0.113(3) Uani 1.00 d . . . C(32) C 0.3700(9) 0.3953(8) -0.537(1) 0.216(6) Uani 1.00 d . . . C(33) C 0.335(1) 0.4571(9) -0.665(1) 0.239(7) Uani 1.00 d . . . C(34) C 0.4571(9) 0.4263(6) -0.7601(10) 0.134(4) Uani 1.00 d . . . H(1) H 0.9313 -0.0939 0.1807 0.0826 Uiso 1.00 calc . . . H(2) H 1.136(6) -0.121(4) 0.362(7) 0.11(2) Uiso 1.00 calc . . . H(3) H 1.238(6) 0.003(4) 0.391(6) 0.09(1) Uiso 1.00 calc . . . H(4) H 1.1031 0.1363 0.3159 0.0791 Uiso 1.00 calc . . . H(5) H 0.453(5) 0.370(3) -0.196(5) 0.06(1) Uiso 1.00 calc . . . H(6) H 0.249(6) 0.177(3) -0.300(6) 0.09(1) Uiso 1.00 calc . . . H(7) H 0.432(5) 0.094(3) -0.107(5) 0.05(1) Uiso 1.00 calc . . . H(8) H 0.776(5) 0.366(3) 0.171(5) 0.04(1) Uiso 1.00 calc . . . H(9) H 0.902(5) 0.478(3) 0.159(6) 0.08(1) Uiso 1.00 calc . . . H(10) H 1.122(5) 0.428(3) 0.070(6) 0.07(1) Uiso 1.00 calc . . . H(11) H 1.238(6) 0.287(3) 0.048(6) 0.09(1) Uiso 1.00 calc . . . H(12) H 1.116(4) 0.188(3) 0.043(5) 0.03(1) Uiso 1.00 calc . . . H(13) H 0.4330 0.0684 0.1780 0.0328 Uiso 1.00 calc . . . H(14) H 0.4110 0.0950 0.4517 0.0942 Uiso 1.00 calc . . . H(15) H 0.5516 0.1644 0.5834 0.0985 Uiso 1.00 calc . . . H(16) H 0.083(6) 0.352(4) -0.543(7) 0.09(1) Uiso 1.00 calc . . . H(17) H 0.163(7) 0.239(4) -0.482(8) 0.09(2) Uiso 1.00 calc . . . H(18) H -0.0118 0.3843 -0.3412 0.1887 Uiso 1.00 calc . . . H(19) H 0.0486 0.2946 -0.2639 0.1887 Uiso 1.00 calc . . . H(20) H -0.1498 0.3366 -0.5068 0.1966 Uiso 1.00 calc . . . H(21) H -0.0803 0.2430 -0.4484 0.1966 Uiso 1.00 calc . . . H(22) H -0.2412 0.3718 -0.2865 0.1469 Uiso 1.00 calc . . . H(23) H -0.1725 0.2779 -0.2290 0.1469 Uiso 1.00 calc . . . H(24) H -0.2916 0.2981 -0.3618 0.1469 Uiso 1.00 calc . . . H(25) H 0.2847 0.4448 -0.3402 0.1352 Uiso 1.00 calc . . . H(26) H 0.1659 0.4502 -0.4701 0.1352 Uiso 1.00 calc . . . H(27) H 0.4567 0.3918 -0.4888 0.2616 Uiso 1.00 calc . . . H(28) H 0.3704 0.3410 -0.5847 0.2616 Uiso 1.00 calc . . . H(29) H 0.3339 0.5157 -0.6258 0.3073 Uiso 1.00 calc . . . H(30) H 0.2470 0.4651 -0.7214 0.3073 Uiso 1.00 calc . . . H(31) H 0.5310 0.4487 -0.7250 0.1608 Uiso 1.00 calc . . . H(32) H 0.4882 0.3653 -0.7523 0.1608 Uiso 1.00 calc . . . H(33) H 0.4241 0.4432 -0.8615 0.1608 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 S(1) 0.103(2) 0.148(2) 0.067(1) -0.045(1) 0.020(1) -0.010(1) O(1) 0.066(3) 0.068(3) 0.085(3) -0.026(2) 0.012(2) -0.021(2) O(2) 0.045(2) 0.059(3) 0.055(2) -0.019(2) 0.003(2) 0.012(2) N(1) 0.063(4) 0.119(5) 0.065(4) -0.009(3) -0.006(2) 0.026(3) C(1) 0.052(3) 0.059(3) 0.049(4) -0.019(2) 0.014(2) 0.001(3) C(2) 0.040(3) 0.054(3) 0.063(4) -0.016(2) 0.016(2) 0.004(3) C(3) 0.068(4) 0.053(3) 0.085(5) -0.013(3) 0.002(3) -0.002(3) C(4) 0.065(5) 0.072(5) 0.119(6) -0.004(4) -0.015(4) 0.015(5) C(5) 0.050(4) 0.083(4) 0.109(6) -0.015(4) -0.007(4) 0.018(4) C(6) 0.062(4) 0.083(4) 0.051(4) -0.031(3) -0.004(3) 0.013(3) C(7) 0.047(3) 0.057(3) 0.051(4) -0.021(3) 0.015(2) 0.004(3) C(8) 0.038(3) 0.056(3) 0.043(3) -0.018(2) 0.012(2) -0.014(2) C(9) 0.037(3) 0.053(3) 0.044(3) -0.010(2) 0.011(2) 0.006(2) C(10) 0.042(3) 0.069(4) 0.042(3) -0.017(3) 0.012(2) 0.003(3) C(11) 0.045(3) 0.071(5) 0.048(4) -0.010(3) 0.011(2) 0.011(3) C(12) 0.042(3) 0.111(5) 0.038(3) -0.019(3) 0.016(2) 0.001(3) C(13) 0.045(4) 0.115(5) 0.042(4) -0.032(4) 0.011(3) -0.005(3) C(14) 0.053(4) 0.074(5) 0.049(4) -0.031(3) 0.017(2) -0.004(3) C(15) 0.046(3) 0.071(4) 0.043(3) -0.023(3) 0.009(2) 0.006(3) C(16) 0.039(3) 0.057(3) 0.048(3) -0.022(2) 0.008(2) 0.004(3) C(17) 0.048(3) 0.058(3) 0.036(3) -0.024(2) 0.005(3) 0.005(3) C(18) 0.052(4) 0.062(3) 0.060(4) -0.013(3) 0.006(3) -0.001(3) C(19) 0.093(5) 0.067(5) 0.071(4) -0.044(4) 0.005(4) 0.011(4) C(20) 0.097(5) 0.091(4) 0.063(4) -0.063(4) 0.004(4) 0.006(4) C(21) 0.060(5) 0.099(4) 0.060(4) -0.050(4) 0.015(3) 0.005(4) C(22) 0.053(3) 0.067(5) 0.045(4) -0.016(3) 0.010(3) -0.004(3) C(23) 0.041(3) 0.052(4) 0.061(2) -0.009(2) 0.025(2) 0.009(3) C(24) 0.024(3) 0.045(3) 0.022(2) -0.023(2) 0.008(2) -0.016(2) C(25) 0.080(5) 0.122(6) 0.039(3) -0.031(4) 0.023(3) 0.002(4) C(26) 0.083(5) 0.121(7) 0.032(4) -0.010(4) 0.012(3) -0.014(3) C(27) 0.054(5) 0.21(1) 0.069(5) -0.059(6) -0.022(3) 0.048(6) C(28) 0.065(5) 0.32(1) 0.095(7) -0.047(7) 0.012(4) 0.087(7) C(29) 0.074(6) 0.32(1) 0.099(7) -0.045(7) 0.018(4) 0.050(8) C(30) 0.072(6) 0.190(9) 0.113(7) -0.034(6) 0.037(4) 0.016(6) C(31) 0.049(4) 0.097(5) 0.158(8) 0.026(4) -0.014(4) 0.030(5) C(32) 0.059(6) 0.32(2) 0.24(1) 0.020(8) 0.067(7) 0.12(1) C(33) 0.136(9) 0.46(2) 0.097(8) -0.04(1) 0.042(6) 0.041(9) C(34) 0.123(8) 0.146(8) 0.124(8) -0.015(6) 0.041(5) -0.008(6) #--------------------------------------------------------------------------- #-- _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 S(1) C(23) 1.683(8) . . yes S(1) C(26) 1.676(9) . . yes O(1) C(1) 1.226(8) . . yes O(2) C(9) 1.394(7) . . yes O(2) C(10) 1.406(8) . . yes N(1) C(12) 1.375(9) . . yes N(1) C(27) 1.49(1) . . yes N(1) C(31) 1.45(1) . . yes C(1) C(2) 1.508(9) . . yes C(1) C(16) 1.489(10) . . yes C(2) C(3) 1.360(9) . . yes C(2) C(7) 1.406(9) . . yes C(3) C(4) 1.40(1) . . yes C(4) C(5) 1.38(1) . . yes C(5) C(6) 1.38(1) . . yes C(6) C(7) 1.381(9) . . yes C(7) C(8) 1.520(9) . . yes C(8) C(9) 1.309(8) . . yes C(8) C(17) 1.485(9) . . yes C(9) C(16) 1.511(9) . . yes C(10) C(11) 1.364(9) . . yes C(10) C(15) 1.378(9) . . yes C(11) C(12) 1.393(10) . . yes C(12) C(13) 1.46(1) . . yes C(13) C(14) 1.41(1) . . yes C(14) C(15) 1.353(9) . . yes C(15) C(16) 1.498(9) . . yes C(16) C(23) 1.545(9) . . yes C(17) C(18) 1.369(9) . . yes C(17) C(22) 1.386(9) . . yes C(18) C(19) 1.38(1) . . yes C(19) C(20) 1.38(1) . . yes C(20) C(21) 1.39(1) . . yes C(21) C(22) 1.38(1) . . yes C(23) C(24) 1.523(8) . . yes C(24) C(25) 1.456(9) . . yes C(25) C(26) 1.28(1) . . yes C(27) C(28) 1.62(1) . . yes C(28) C(29) 1.441(9) . . yes C(29) C(30) 1.48(1) . . yes C(31) C(32) 1.605(9) . . yes C(32) C(33) 1.491(10) . . yes C(33) C(34) 1.546(9) . . 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(23) S(1) C(26) 94.2(4) . . . yes C(9) O(2) C(10) 106.5(5) . . . yes C(12) N(1) C(27) 120.4(9) . . . yes C(12) N(1) C(31) 122.2(8) . . . yes C(27) N(1) C(31) 117.3(8) . . . yes O(1) C(1) C(2) 120.4(7) . . . yes O(1) C(1) C(16) 122.9(7) . . . yes C(2) C(1) C(16) 116.1(7) . . . yes C(1) C(2) C(3) 120.0(7) . . . yes C(1) C(2) C(7) 117.7(7) . . . yes C(3) C(2) C(7) 122.0(7) . . . yes C(2) C(3) C(4) 119.5(8) . . . yes C(3) C(4) C(5) 118.7(9) . . . yes C(4) C(5) C(6) 121.5(9) . . . yes C(5) C(6) C(7) 120.3(8) . . . yes C(2) C(7) C(6) 117.8(7) . . . yes C(2) C(7) C(8) 120.3(7) . . . yes C(6) C(7) C(8) 121.7(7) . . . yes C(7) C(8) C(9) 115.1(6) . . . yes C(7) C(8) C(17) 121.7(6) . . . yes C(9) C(8) C(17) 123.2(7) . . . yes O(2) C(9) C(8) 123.2(6) . . . yes O(2) C(9) C(16) 109.6(6) . . . yes C(8) C(9) C(16) 127.0(7) . . . yes O(2) C(10) C(11) 121.9(7) . . . yes O(2) C(10) C(15) 111.9(6) . . . yes C(11) C(10) C(15) 126.3(7) . . . yes C(10) C(11) C(12) 117.6(8) . . . yes N(1) C(12) C(11) 121.4(8) . . . yes N(1) C(12) C(13) 120.6(8) . . . yes C(11) C(12) C(13) 117.9(7) . . . yes C(12) C(13) C(14) 120.2(8) . . . yes C(13) C(14) C(15) 120.3(8) . . . yes C(10) C(15) C(14) 117.8(7) . . . yes C(10) C(15) C(16) 108.2(6) . . . yes C(14) C(15) C(16) 133.8(7) . . . yes C(1) C(16) C(9) 109.3(6) . . . yes C(1) C(16) C(15) 119.9(6) . . . yes C(1) C(16) C(23) 104.1(5) . . . yes C(9) C(16) C(15) 101.0(5) . . . yes C(9) C(16) C(23) 111.9(6) . . . yes C(15) C(16) C(23) 110.8(5) . . . yes C(8) C(17) C(18) 121.2(7) . . . yes C(8) C(17) C(22) 120.9(7) . . . yes C(18) C(17) C(22) 118.0(7) . . . yes C(17) C(18) C(19) 122.3(8) . . . yes C(18) C(19) C(20) 119.0(10) . . . yes C(19) C(20) C(21) 119.7(9) . . . yes C(20) C(21) C(22) 119.8(9) . . . yes C(17) C(22) C(21) 121.2(8) . . . yes S(1) C(23) C(16) 121.0(5) . . . yes S(1) C(23) C(24) 112.1(4) . . . yes C(16) C(23) C(24) 126.9(6) . . . yes C(23) C(24) C(25) 101.1(5) . . . yes C(24) C(25) C(26) 121.9(7) . . . yes S(1) C(26) C(25) 110.7(6) . . . yes N(1) C(27) C(28) 103.8(9) . . . yes C(27) C(28) C(29) 112.5(10) . . . yes C(28) C(29) C(30) 112(1) . . . yes N(1) C(31) C(32) 103.9(9) . . . yes C(31) C(32) C(33) 113.5(9) . . . yes C(32) C(33) C(34) 105(1) . . . yes #--------------------------------------------------------------------------- #-- #===============================================END data_3a _database_code_depnum_ccdc_archive 'CCDC 605728' _audit_creation_date 'Tue Jan 3 04:41:57 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #--------------------------------------------------------------------------- #-- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------------- #-- _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 493.69 _chemical_formula_analytical ? _chemical_formula_sum ' C34 H39 N O2 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_melting_point ? #--------------------------------------------------------------------------- #-- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 9.471(5) _cell_length_b 30.489(6) _cell_length_c 10.734(5) _cell_angle_alpha 90 _cell_angle_beta 114.03(3) _cell_angle_gamma 90 _cell_volume 2830(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 12.3 _cell_measurement_temperature 296.2 #--------------------------------------------------------------------------- #-- _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.071 _exptl_crystal_F_000 1064.00 _exptl_absorpt_correction_T_min 0.969 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #--------------------------------------------------------------------------- #-- _diffrn_special_details ; ? ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 5417 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 0.9992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.9992 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.71 _reflns_number_total 4981 _reflns_number_gt 2071 _reflns_threshold_expression F^2^>2.0\s(F^2^) _diffrn_orient_matrix_UB_11 0.081120 _diffrn_orient_matrix_UB_12 -0.007210 _diffrn_orient_matrix_UB_13 0.092280 _diffrn_orient_matrix_UB_21 0.011860 _diffrn_orient_matrix_UB_22 0.031900 _diffrn_orient_matrix_UB_23 0.023740 _diffrn_orient_matrix_UB_31 -0.081500 _diffrn_orient_matrix_UB_32 -0.002530 _diffrn_orient_matrix_UB_33 0.036400 #--------------------------------------------------------------------------- #-- _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 4981 _refine_ls_number_parameters 459 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.04000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_R_factor_all 0.11358 _refine_ls_R_factor_gt 0.05277 _refine_ls_wR_factor_ref 0.16084 _refine_ls_wR_factor_gt 0.11710 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_shift/su_max 0.0047 _refine_diff_density_max 0.21 _refine_diff_density_min -0.22 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.005(1) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H H 0.000 0.000 'International Tables Vol C Table 6.1.1.2' N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' #--------------------------------------------------------------------------- #-- 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_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.1433(3) 0.03253(9) 0.4084(3) 0.084(1) Uani 1.00 d . . . O(2) O 0.3674(2) 0.12722(7) 0.7759(2) 0.0470(7) Uani 1.00 d . . . N(1) N 0.3248(3) 0.28121(9) 0.8168(3) 0.059(1) Uani 1.00 d . . . C(1) C 0.2108(5) 0.0461(1) 0.5260(4) 0.059(1) Uani 1.00 d . . . C(2) C 0.3464(4) 0.0254(1) 0.6347(4) 0.053(1) Uani 1.00 d . . . C(3) C 0.4307(6) -0.0108(1) 0.6270(5) 0.068(2) Uani 1.00 d . . . C(4) C 0.5586(6) -0.0222(1) 0.7405(5) 0.072(2) Uani 1.00 d . . . C(5) C 0.6017(5) 0.0007(1) 0.8615(5) 0.061(1) Uani 1.00 d . . . C(6) C 0.5163(4) 0.0367(1) 0.8704(4) 0.054(1) Uani 1.00 d . . . C(7) C 0.3899(4) 0.0491(1) 0.7558(4) 0.046(1) Uani 1.00 d . . . C(8) C 0.2786(4) 0.08687(10) 0.7364(3) 0.0441(10) Uani 1.00 d . . . C(9) C 0.2799(4) 0.1643(1) 0.7250(3) 0.043(1) Uani 1.00 d . . . C(10) C 0.3409(4) 0.2026(1) 0.7933(4) 0.046(1) Uani 1.00 d . . . C(11) C 0.2649(4) 0.2427(1) 0.7494(4) 0.049(1) Uani 1.00 d . . . C(12) C 0.1213(4) 0.2417(1) 0.6340(4) 0.057(1) Uani 1.00 d . . . C(13) C 0.0675(5) 0.2034(1) 0.5660(4) 0.059(1) Uani 1.00 d . . . C(14) C 0.1448(4) 0.1632(1) 0.6055(3) 0.047(1) Uani 1.00 d . . . C(15) C 0.1079(4) 0.1232(1) 0.5240(3) 0.052(1) Uani 1.00 d . . . C(16) C 0.1808(4) 0.0864(1) 0.5857(3) 0.049(1) Uani 1.00 d . . . C(17) C 0.1860(4) 0.0805(1) 0.8230(3) 0.047(1) Uani 1.00 d . . . C(18) C 0.2181(5) 0.1033(1) 0.9425(4) 0.056(1) Uani 1.00 d . . . C(19) C 0.1311(6) 0.0959(1) 1.0186(5) 0.076(2) Uani 1.00 d . . . C(20) C 0.0133(6) 0.0653(2) 0.9752(6) 0.080(2) Uani 1.00 d . . . C(21) C -0.0175(6) 0.0426(2) 0.8571(6) 0.077(2) Uani 1.00 d . . . C(22) C 0.0662(5) 0.0502(1) 0.7801(4) 0.060(1) Uani 1.00 d . . . C(23) C -0.0003(5) 0.1238(2) 0.3744(4) 0.065(1) Uani 1.00 d . . . C(24) C -0.1594(6) 0.1067(2) 0.3492(4) 0.084(2) Uani 1.00 d . . . C(25) C -0.2683(6) 0.1024(2) 0.2001(5) 0.110(2) Uani 1.00 d . . . C(26) C -0.3200(8) 0.1419(2) 0.1305(6) 0.172(3) Uani 1.00 d . . . C(27) C 0.2406(6) 0.3229(1) 0.7781(5) 0.066(2) Uani 1.00 d . . . C(28) C 0.2690(6) 0.3477(1) 0.6681(5) 0.071(2) Uani 1.00 d . . . C(29) C 0.1587(7) 0.3862(2) 0.6134(7) 0.086(2) Uani 1.00 d . . . C(30) C 0.0065(8) 0.3728(2) 0.5082(7) 0.098(2) Uani 1.00 d . . . C(31) C 0.4882(5) 0.2843(1) 0.9101(4) 0.061(1) Uani 1.00 d . . . C(32) C 0.5211(6) 0.2771(2) 1.0575(5) 0.074(2) Uani 1.00 d . . . C(33) C 0.6936(6) 0.2785(2) 1.1470(6) 0.100(2) Uani 1.00 d . . . C(34) C 0.7334(8) 0.2712(2) 1.2937(6) 0.166(3) Uani 1.00 d . . . H(1) H 0.396(4) -0.025(1) 0.537(4) 0.07(1) Uiso 1.00 calc . . . H(2) H 0.618(4) -0.046(1) 0.741(4) 0.07(1) Uiso 1.00 calc . . . H(3) H 0.687(4) -0.008(1) 0.945(3) 0.06(1) Uiso 1.00 calc . . . H(4) H 0.545(4) 0.052(1) 0.960(4) 0.07(1) Uiso 1.00 calc . . . H(5) H 0.428(4) 0.2014(10) 0.872(3) 0.049(10) Uiso 1.00 calc . . . H(6) H 0.068(4) 0.269(1) 0.607(3) 0.06(1) Uiso 1.00 calc . . . H(7) H -0.028(3) 0.2049(8) 0.487(3) 0.033(8) Uiso 1.00 calc . . . H(8) H 0.298(3) 0.1250(9) 0.968(3) 0.032(8) Uiso 1.00 calc . . . H(9) H 0.158(4) 0.111(1) 1.103(4) 0.07(1) Uiso 1.00 calc . . . H(10) H -0.047(5) 0.060(1) 1.028(4) 0.10(2) Uiso 1.00 calc . . . H(11) H -0.104(5) 0.022(1) 0.824(4) 0.08(1) Uiso 1.00 calc . . . H(12) H 0.029(4) 0.034(1) 0.689(4) 0.09(1) Uiso 1.00 calc . . . H(13) H 0.042(5) 0.109(1) 0.320(4) 0.10(2) Uiso 1.00 calc . . . H(14) H -0.004(4) 0.152(1) 0.342(4) 0.08(1) Uiso 1.00 calc . . . H(15) H -0.131(6) 0.077(2) 0.392(5) 0.13(2) Uiso 1.00 calc . . . H(16) H -0.215(6) 0.127(2) 0.391(5) 0.14(2) Uiso 1.00 calc . . . H(17) H -0.2158 0.0858 0.1546 0.1308 Uiso 1.00 calc . . . H(18) H -0.3563 0.0854 0.1939 0.1308 Uiso 1.00 calc . . . H(19) H -0.3863 0.1389 0.0378 0.2002 Uiso 1.00 calc . . . H(20) H -0.3721 0.1598 0.1742 0.2002 Uiso 1.00 calc . . . H(21) H -0.2316 0.1601 0.1349 0.2002 Uiso 1.00 calc . . . H(22) H 0.130(4) 0.318(1) 0.744(3) 0.07(1) Uiso 1.00 calc . . . H(23) H 0.276(4) 0.342(1) 0.863(4) 0.07(1) Uiso 1.00 calc . . . H(24) H 0.254(4) 0.325(1) 0.587(3) 0.06(1) Uiso 1.00 calc . . . H(25) H 0.378(4) 0.356(1) 0.705(4) 0.07(1) Uiso 1.00 calc . . . H(26) H 0.149(5) 0.401(1) 0.695(4) 0.10(2) Uiso 1.00 calc . . . H(27) H 0.210(5) 0.408(1) 0.571(4) 0.11(2) Uiso 1.00 calc . . . H(28) H -0.053(6) 0.350(2) 0.537(5) 0.14(2) Uiso 1.00 calc . . . H(29) H 0.012(6) 0.359(2) 0.423(5) 0.13(2) Uiso 1.00 calc . . . H(30) H -0.071(6) 0.396(2) 0.467(5) 0.12(2) Uiso 1.00 calc . . . H(31) H 0.543(3) 0.264(1) 0.885(3) 0.044(10) Uiso 1.00 calc . . . H(32) H 0.529(4) 0.317(1) 0.901(4) 0.09(1) Uiso 1.00 calc . . . H(33) H 0.479(4) 0.249(1) 1.068(3) 0.06(1) Uiso 1.00 calc . . . H(34) H 0.480(5) 0.301(1) 1.094(4) 0.11(2) Uiso 1.00 calc . . . H(35) H 0.745(6) 0.257(2) 1.121(5) 0.12(2) Uiso 1.00 calc . . . H(36) H 0.753(7) 0.308(2) 1.148(7) 0.20(3) Uiso 1.00 calc . . . H(37) H 0.6959 0.2419 1.3065 0.1876 Uiso 1.00 calc . . . H(38) H 0.8408 0.2715 1.3462 0.1876 Uiso 1.00 calc . . . H(39) H 0.6837 0.2917 1.3289 0.1876 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) 0.096(2) 0.080(2) 0.060(2) -0.011(2) 0.016(2) -0.024(2) O(2) 0.047(1) 0.036(1) 0.049(1) -0.005(1) 0.011(1) -0.001(1) N(1) 0.061(2) 0.038(2) 0.070(2) -0.003(2) 0.018(2) 0.000(2) C(1) 0.070(3) 0.049(2) 0.059(3) -0.020(2) 0.027(2) -0.015(2) C(2) 0.060(3) 0.044(2) 0.060(2) -0.004(2) 0.030(2) -0.005(2) C(3) 0.084(3) 0.056(3) 0.071(3) -0.009(2) 0.039(3) -0.013(2) C(4) 0.087(4) 0.049(3) 0.096(4) 0.007(3) 0.055(3) -0.006(3) C(5) 0.060(3) 0.050(2) 0.075(3) 0.006(2) 0.028(3) 0.008(2) C(6) 0.059(3) 0.044(2) 0.060(3) 0.001(2) 0.026(2) 0.002(2) C(7) 0.048(2) 0.037(2) 0.055(2) -0.007(2) 0.023(2) 0.001(2) C(8) 0.046(2) 0.033(2) 0.046(2) -0.004(2) 0.010(2) -0.002(2) C(9) 0.044(2) 0.036(2) 0.046(2) -0.002(2) 0.016(2) 0.004(2) C(10) 0.044(2) 0.042(2) 0.048(2) -0.002(2) 0.014(2) 0.004(2) C(11) 0.052(2) 0.040(2) 0.055(2) -0.003(2) 0.022(2) 0.003(2) C(12) 0.058(3) 0.044(2) 0.060(3) 0.007(2) 0.015(2) 0.012(2) C(13) 0.050(3) 0.064(3) 0.048(2) 0.000(2) 0.006(2) 0.009(2) C(14) 0.041(2) 0.047(2) 0.046(2) -0.003(2) 0.011(2) 0.005(2) C(15) 0.047(2) 0.060(2) 0.046(2) -0.012(2) 0.016(2) -0.003(2) C(16) 0.052(2) 0.045(2) 0.042(2) -0.010(2) 0.011(2) -0.005(2) C(17) 0.052(2) 0.038(2) 0.050(2) 0.005(2) 0.019(2) 0.005(2) C(18) 0.069(3) 0.042(2) 0.064(3) -0.003(2) 0.033(2) -0.002(2) C(19) 0.118(4) 0.057(3) 0.072(3) 0.016(3) 0.059(3) 0.003(2) C(20) 0.090(4) 0.066(3) 0.119(5) 0.012(3) 0.076(4) 0.024(3) C(21) 0.069(3) 0.071(3) 0.099(4) -0.006(3) 0.044(3) 0.005(3) C(22) 0.052(2) 0.061(3) 0.065(3) -0.009(2) 0.021(2) 0.003(2) C(23) 0.072(3) 0.070(3) 0.044(3) -0.016(3) 0.013(2) 0.001(2) C(24) 0.059(3) 0.120(5) 0.049(3) -0.023(3) -0.001(2) -0.004(3) C(25) 0.086(4) 0.151(5) 0.068(3) -0.036(3) 0.004(3) -0.010(3) C(26) 0.177(7) 0.147(6) 0.109(5) -0.032(5) -0.027(5) 0.041(4) C(27) 0.081(4) 0.045(2) 0.078(3) 0.004(2) 0.038(3) 0.002(2) C(28) 0.075(3) 0.057(3) 0.093(4) 0.006(2) 0.047(3) 0.015(3) C(29) 0.102(4) 0.055(3) 0.112(4) 0.020(3) 0.056(4) 0.031(3) C(30) 0.089(4) 0.109(5) 0.100(5) 0.036(4) 0.044(4) 0.026(4) C(31) 0.065(3) 0.042(2) 0.076(3) -0.006(2) 0.028(2) -0.009(2) C(32) 0.081(4) 0.069(3) 0.071(3) 0.007(3) 0.030(3) -0.010(3) C(33) 0.072(4) 0.114(5) 0.093(4) 0.021(4) 0.013(3) -0.009(4) C(34) 0.149(6) 0.200(7) 0.093(5) 0.075(5) -0.010(4) -0.014(5) #--------------------------------------------------------------------------- #-- _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) 1.231(4) . . yes O(2) C(8) 1.452(4) . . yes O(2) C(9) 1.377(4) . . yes N(1) C(11) 1.374(4) . . yes N(1) C(27) 1.467(5) . . yes N(1) C(31) 1.464(5) . . yes C(1) C(2) 1.479(5) . . yes C(1) C(16) 1.465(5) . . yes C(2) C(3) 1.385(5) . . yes C(2) C(7) 1.395(4) . . yes C(3) C(4) 1.368(6) . . yes C(4) C(5) 1.381(6) . . yes C(5) C(6) 1.388(5) . . yes C(6) C(7) 1.375(5) . . yes C(7) C(8) 1.517(4) . . yes C(8) C(16) 1.502(4) . . yes C(8) C(17) 1.528(4) . . yes C(9) C(10) 1.375(4) . . yes C(9) C(14) 1.395(4) . . yes C(10) C(11) 1.400(5) . . yes C(11) C(12) 1.419(5) . . yes C(12) C(13) 1.362(5) . . yes C(13) C(14) 1.403(5) . . yes C(14) C(15) 1.458(4) . . yes C(15) C(16) 1.343(4) . . yes C(15) C(23) 1.513(5) . . yes C(17) C(18) 1.380(5) . . yes C(17) C(22) 1.390(5) . . yes C(18) C(19) 1.395(5) . . yes C(19) C(20) 1.381(6) . . yes C(20) C(21) 1.369(6) . . yes C(21) C(22) 1.378(6) . . yes C(23) C(24) 1.512(6) . . yes C(24) C(25) 1.515(6) . . yes C(25) C(26) 1.396(7) . . yes C(27) C(28) 1.515(6) . . yes C(28) C(29) 1.523(6) . . yes C(29) C(30) 1.481(8) . . yes C(31) C(32) 1.500(6) . . yes C(32) C(33) 1.521(7) . . yes C(33) C(34) 1.479(8) . . 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(2) C(9) 113.4(2) . . . yes C(11) N(1) C(27) 122.0(3) . . . yes C(11) N(1) C(31) 120.6(3) . . . yes C(27) N(1) C(31) 116.1(3) . . . yes O(1) C(1) C(2) 126.0(3) . . . yes O(1) C(1) C(16) 128.1(4) . . . yes C(2) C(1) C(16) 105.8(3) . . . yes C(1) C(2) C(3) 129.0(4) . . . yes C(1) C(2) C(7) 110.3(3) . . . yes C(3) C(2) C(7) 120.6(4) . . . yes C(2) C(3) C(4) 118.2(4) . . . yes C(3) C(4) C(5) 121.6(4) . . . yes C(4) C(5) C(6) 120.4(4) . . . yes C(5) C(6) C(7) 118.4(4) . . . yes C(2) C(7) C(6) 120.7(3) . . . yes C(2) C(7) C(8) 109.9(3) . . . yes C(6) C(7) C(8) 129.5(3) . . . yes O(2) C(8) C(7) 108.4(3) . . . yes O(2) C(8) C(16) 110.7(3) . . . yes O(2) C(8) C(17) 109.7(3) . . . yes C(7) C(8) C(16) 103.3(3) . . . yes C(7) C(8) C(17) 111.1(3) . . . yes C(16) C(8) C(17) 113.5(3) . . . yes O(2) C(9) C(10) 115.6(3) . . . yes O(2) C(9) C(14) 121.5(3) . . . yes C(10) C(9) C(14) 122.7(3) . . . yes C(9) C(10) C(11) 121.1(3) . . . yes N(1) C(11) C(10) 121.6(3) . . . yes N(1) C(11) C(12) 121.5(3) . . . yes C(10) C(11) C(12) 117.0(3) . . . yes C(11) C(12) C(13) 120.2(4) . . . yes C(12) C(13) C(14) 123.6(4) . . . yes C(9) C(14) C(13) 115.2(3) . . . yes C(9) C(14) C(15) 118.6(3) . . . yes C(13) C(14) C(15) 125.6(3) . . . yes C(14) C(15) C(16) 117.0(3) . . . yes C(14) C(15) C(23) 121.3(4) . . . yes C(16) C(15) C(23) 121.6(4) . . . yes C(1) C(16) C(8) 109.6(3) . . . yes C(1) C(16) C(15) 129.6(3) . . . yes C(8) C(16) C(15) 119.4(3) . . . yes C(8) C(17) C(18) 122.6(3) . . . yes C(8) C(17) C(22) 118.4(3) . . . yes C(18) C(17) C(22) 119.0(4) . . . yes C(17) C(18) C(19) 120.3(4) . . . yes C(18) C(19) C(20) 120.1(5) . . . yes C(19) C(20) C(21) 119.6(5) . . . yes C(20) C(21) C(22) 120.8(5) . . . yes C(17) C(22) C(21) 120.3(4) . . . yes C(15) C(23) C(24) 112.4(4) . . . yes C(23) C(24) C(25) 114.8(4) . . . yes C(24) C(25) C(26) 115.5(5) . . . yes N(1) C(27) C(28) 113.9(4) . . . yes C(27) C(28) C(29) 112.0(4) . . . yes C(28) C(29) C(30) 112.5(5) . . . yes N(1) C(31) C(32) 114.8(4) . . . yes C(31) C(32) C(33) 111.7(4) . . . yes C(32) C(33) C(34) 114.2(6) . . . yes #--------------------------------------------------------------------------- #-- #===============================================END data_3b _database_code_depnum_ccdc_archive 'CCDC 605729' _audit_creation_date 'Tue Jan 3 08:05:56 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #--------------------------------------------------------------------------- #-- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------------- #-- _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 513.68 _chemical_formula_analytical ? _chemical_formula_sum ' C36 H35 N O2 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_melting_point ? #--------------------------------------------------------------------------- #-- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21/b 21/c 21/a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z 1/2-x,-y,1/2+z -x,-y,-z 1/2-x,1/2+y,z x,1/2-y,1/2+z 1/2+x,y,1/2-z _cell_length_a 20.947(7) _cell_length_b 31.759(7) _cell_length_c 8.758(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5826(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 12 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 11.9 _cell_measurement_temperature 296.2 #--------------------------------------------------------------------------- #-- _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.071 _exptl_crystal_F_000 2192.00 _exptl_absorpt_correction_T_min 0.951 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #--------------------------------------------------------------------------- #-- _diffrn_special_details ; ? ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 5385 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 0.9309 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 00.9309 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.54 _reflns_number_total 4786 _reflns_number_gt 1284 _reflns_threshold_expression F^2^>2.0\s(F^2^) _diffrn_orient_matrix_UB_11 0.033940 _diffrn_orient_matrix_UB_12 0.021800 _diffrn_orient_matrix_UB_13 0.014200 _diffrn_orient_matrix_UB_21 0.033190 _diffrn_orient_matrix_UB_22 -0.022620 _diffrn_orient_matrix_UB_23 -0.002910 _diffrn_orient_matrix_UB_31 -0.005110 _diffrn_orient_matrix_UB_32 -0.002150 _diffrn_orient_matrix_UB_33 -0.113260 #--------------------------------------------------------------------------- _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 4786 _refine_ls_number_parameters 465 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.04000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_R_factor_all 0.19307 _refine_ls_R_factor_gt 0.05528 _refine_ls_wR_factor_ref 0.18927 _refine_ls_wR_factor_gt 0.10825 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_shift/su_max 0.0028 _refine_diff_density_max 0.83 _refine_diff_density_min -0.87 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0016(3) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H H 0.000 0.000 'International Tables Vol C Table 6.1.1.2' N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' #--------------------------------------------------------------------------- #-- 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_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 1.0263(2) 0.0275(1) 0.2637(6) 0.090(2) Uani 1.00 d . . . O(2) O 0.8589(2) 0.1217(1) 0.2286(4) 0.048(1) Uani 1.00 d . . . N(1) N 0.8541(3) 0.2705(2) 0.1525(6) 0.057(2) Uani 1.00 d . . . C(1) C 0.9730(3) 0.0416(2) 0.2442(8) 0.063(2) Uani 1.00 d . . . C(2) C 0.9128(3) 0.0224(2) 0.2974(7) 0.060(2) Uani 1.00 d . . . C(3) C 0.9039(5) -0.0140(2) 0.3850(9) 0.074(3) Uani 1.00 d . . . C(4) C 0.8435(6) -0.0253(3) 0.4202(10) 0.086(3) Uani 1.00 d . . . C(5) C 0.7910(4) -0.0029(3) 0.374(1) 0.079(3) Uani 1.00 d . . . C(6) C 0.7989(3) 0.0330(2) 0.2829(8) 0.063(2) Uani 1.00 d . . . C(7) C 0.8601(3) 0.0455(2) 0.2499(7) 0.052(2) Uani 1.00 d . . . C(8) C 0.8815(3) 0.0832(2) 0.1559(7) 0.046(2) Uani 1.00 d . . . C(9) C 0.8900(3) 0.1576(2) 0.1731(7) 0.047(2) Uani 1.00 d . . . C(10) C 0.8570(3) 0.1945(2) 0.1839(7) 0.044(2) Uani 1.00 d . . . C(11) C 0.8855(3) 0.2324(2) 0.1369(7) 0.051(2) Uani 1.00 d . . . C(12) C 0.9466(3) 0.2302(2) 0.0689(8) 0.053(2) Uani 1.00 d . . . C(13) C 0.9785(3) 0.1925(2) 0.0656(8) 0.054(2) Uani 1.00 d . . . C(14) C 0.9526(3) 0.1549(2) 0.1207(7) 0.049(2) Uani 1.00 d . . . C(15) C 0.9883(3) 0.1159(2) 0.1382(7) 0.049(2) Uani 1.00 d . . . C(16) C 0.9534(3) 0.0813(2) 0.1681(7) 0.048(2) Uani 1.00 d . . . C(17) C 0.8574(3) 0.0809(2) -0.0073(7) 0.047(2) Uani 1.00 d . . . C(18) C 0.8054(3) 0.1041(2) -0.0562(9) 0.053(2) Uani 1.00 d . . . C(19) C 0.7851(4) 0.1010(2) -0.206(1) 0.069(3) Uani 1.00 d . . . C(20) C 0.8154(4) 0.0746(3) -0.3073(10) 0.077(3) Uani 1.00 d . . . C(21) C 0.8655(4) 0.0508(2) -0.256(1) 0.073(3) Uani 1.00 d . . . C(22) C 0.8862(4) 0.0540(2) -0.1098(9) 0.065(3) Uani 1.00 d . . . C(23) C 1.0597(3) 0.1172(2) 0.1345(8) 0.058(2) Uani 1.00 d . . . C(24) C 1.0939(4) 0.1452(3) 0.2201(10) 0.080(3) Uani 1.00 d . . . C(25) C 1.1600(4) 0.1459(3) 0.214(1) 0.093(4) Uani 1.00 d . . . C(26) C 1.1917(4) 0.1188(4) 0.120(1) 0.110(4) Uani 1.00 d . . . C(27) C 1.1592(4) 0.0901(3) 0.040(1) 0.095(4) Uani 1.00 d . . . C(28) C 1.0922(4) 0.0887(3) 0.044(1) 0.077(3) Uani 1.00 d . . . C(29) C 0.8799(4) 0.3093(2) 0.0849(9) 0.062(3) Uani 1.00 d . . . C(30) C 0.9329(4) 0.3306(2) 0.1756(10) 0.068(3) Uani 1.00 d . . . C(31) C 0.9690(5) 0.3610(3) 0.074(1) 0.109(4) Uani 1.00 d . . . C(32) C 1.0229(6) 0.3806(3) 0.153(1) 0.188(6) Uani 1.00 d . . . C(33) C 0.7993(4) 0.2752(2) 0.2495(10) 0.065(3) Uani 1.00 d . . . C(34) C 0.7356(4) 0.2720(3) 0.168(1) 0.078(3) Uani 1.00 d . . . C(35) C 0.6793(5) 0.2778(4) 0.271(1) 0.113(5) Uani 1.00 d . . . C(36) C 0.6175(4) 0.2747(4) 0.191(1) 0.179(5) Uani 1.00 d . . . H(1) H 0.945(3) -0.028(2) 0.415(8) 0.11(3) Uiso 1.00 calc . . . H(2) H 0.837(2) -0.049(2) 0.489(5) 0.04(2) Uiso 1.00 calc . . . H(3) H 0.751(3) -0.010(2) 0.375(7) 0.06(2) Uiso 1.00 calc . . . H(4) H 0.7627 0.0482 0.2486 0.0723 Uiso 1.00 calc . . . H(5) H 0.815(2) 0.196(1) 0.219(5) 0.04(2) Uiso 1.00 calc . . . H(6) H 0.966(2) 0.253(2) 0.035(7) 0.08(2) Uiso 1.00 calc . . . H(7) H 1.021(3) 0.191(2) 0.012(6) 0.07(2) Uiso 1.00 calc . . . H(8) H 0.784(2) 0.122(1) 0.010(5) 0.04(2) Uiso 1.00 calc . . . H(9) H 0.743(3) 0.118(2) -0.241(7) 0.09(2) Uiso 1.00 calc . . . H(10) H 0.800(2) 0.074(2) -0.411(6) 0.06(2) Uiso 1.00 calc . . . H(11) H 0.894(3) 0.032(2) -0.323(8) 0.12(3) Uiso 1.00 calc . . . H(12) H 0.920(2) 0.040(2) -0.073(6) 0.05(2) Uiso 1.00 calc . . . H(13) H 1.074(2) 0.161(1) 0.301(5) 0.03(2) Uiso 1.00 calc . . . H(14) H 1.184(3) 0.169(2) 0.275(8) 0.11(3) Uiso 1.00 calc . . . H(15) H 1.239(3) 0.123(2) 0.133(7) 0.11(3) Uiso 1.00 calc . . . H(16) H 1.178(3) 0.075(2) -0.043(6) 0.08(2) Uiso 1.00 calc . . . H(17) H 1.070(3) 0.072(2) -0.011(7) 0.06(3) Uiso 1.00 calc . . . H(18) H 0.843(4) 0.329(2) 0.063(9) 0.15(4) Uiso 1.00 calc . . . H(19) H 0.899(2) 0.301(1) -0.019(6) 0.05(2) Uiso 1.00 calc . . . H(20) H 0.911(3) 0.347(2) 0.260(7) 0.07(2) Uiso 1.00 calc . . . H(21) H 0.962(2) 0.308(2) 0.223(6) 0.05(2) Uiso 1.00 calc . . . H(22) H 0.991(4) 0.346(2) -0.026(10) 0.15(4) Uiso 1.00 calc . . . H(23) H 0.936(5) 0.388(3) 0.06(1) 0.25(6) Uiso 1.00 calc . . . H(24) H 1.0428 0.3992 0.0818 0.2131 Uiso 1.00 calc . . . H(25) H 1.0090 0.3941 0.2383 0.2131 Uiso 1.00 calc . . . H(26) H 1.0525 0.3584 0.1767 0.2131 Uiso 1.00 calc . . . H(27) H 0.800(3) 0.304(2) 0.306(7) 0.09(2) Uiso 1.00 calc . . . H(28) H 0.803(2) 0.256(1) 0.335(5) 0.03(1) Uiso 1.00 calc . . . H(29) H 0.730(3) 0.243(2) 0.112(9) 0.14(4) Uiso 1.00 calc . . . H(30) H 0.739(3) 0.297(2) 0.103(7) 0.08(2) Uiso 1.00 calc . . . H(31) H 0.676(3) 0.311(2) 0.330(8) 0.12(3) Uiso 1.00 calc . . . H(32) H 0.677(4) 0.255(3) 0.34(1) 0.15(5) Uiso 1.00 calc . . . H(33) H 0.6175 0.2458 0.1333 0.2077 Uiso 1.00 calc . . . H(34) H 0.5826 0.2731 0.2541 0.2077 Uiso 1.00 calc . . . H(35) H 0.6132 0.2942 0.1120 0.2077 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) 0.069(3) 0.082(3) 0.119(4) 0.029(3) -0.010(3) 0.023(3) O(2) 0.039(2) 0.048(2) 0.056(3) 0.002(2) 0.004(2) -0.008(2) N(1) 0.064(4) 0.049(4) 0.058(4) 0.003(3) 0.005(3) -0.005(3) C(1) 0.059(5) 0.062(5) 0.067(5) 0.008(4) -0.004(5) 0.004(4) C(2) 0.075(5) 0.053(5) 0.053(5) 0.002(4) -0.003(4) 0.003(4) C(3) 0.081(7) 0.061(6) 0.081(6) 0.010(5) 0.000(5) 0.003(5) C(4) 0.126(9) 0.054(5) 0.079(6) -0.006(6) 0.018(6) 0.007(5) C(5) 0.071(7) 0.064(6) 0.101(7) -0.014(6) 0.006(6) -0.012(5) C(6) 0.072(5) 0.046(4) 0.073(5) -0.011(4) 0.008(4) -0.008(4) C(7) 0.066(5) 0.040(4) 0.050(4) -0.005(4) 0.004(4) -0.007(4) C(8) 0.047(4) 0.046(4) 0.044(4) 0.006(3) -0.005(3) -0.013(4) C(9) 0.037(4) 0.054(4) 0.049(4) 0.000(4) -0.005(3) -0.009(4) C(10) 0.030(4) 0.050(4) 0.052(4) 0.007(4) -0.001(4) -0.012(3) C(11) 0.054(4) 0.046(4) 0.053(4) 0.004(4) -0.006(4) -0.005(4) C(12) 0.055(5) 0.045(4) 0.059(5) -0.003(4) 0.010(4) 0.011(4) C(13) 0.035(4) 0.066(5) 0.060(5) 0.000(4) 0.008(4) -0.003(4) C(14) 0.044(4) 0.048(4) 0.054(5) -0.005(4) -0.002(3) 0.000(4) C(15) 0.046(4) 0.049(4) 0.051(4) 0.007(4) -0.007(4) -0.010(4) C(16) 0.043(4) 0.044(4) 0.056(4) 0.005(3) -0.010(3) -0.008(4) C(17) 0.041(4) 0.041(4) 0.059(4) 0.002(3) 0.004(4) -0.009(4) C(18) 0.055(5) 0.031(4) 0.074(6) 0.005(4) -0.003(4) -0.012(4) C(19) 0.070(6) 0.057(5) 0.082(7) -0.005(4) -0.024(5) -0.004(5) C(20) 0.092(7) 0.085(6) 0.053(6) -0.011(5) -0.023(5) 0.000(5) C(21) 0.066(6) 0.084(6) 0.068(6) 0.007(5) -0.008(5) -0.019(5) C(22) 0.055(5) 0.070(6) 0.071(6) 0.008(4) -0.016(5) -0.010(5) C(23) 0.042(4) 0.063(5) 0.069(5) 0.007(4) 0.000(4) 0.001(4) C(24) 0.049(6) 0.107(7) 0.085(7) 0.006(5) 0.004(5) -0.016(6) C(25) 0.046(6) 0.088(7) 0.146(9) -0.008(5) -0.015(6) 0.003(7) C(26) 0.040(6) 0.111(9) 0.18(1) -0.002(6) -0.005(8) 0.028(8) C(27) 0.058(7) 0.116(8) 0.112(8) 0.031(6) 0.030(6) 0.007(7) C(28) 0.054(6) 0.084(7) 0.093(7) 0.011(5) 0.006(5) -0.004(6) C(29) 0.075(6) 0.059(5) 0.053(5) -0.002(5) 0.000(5) 0.006(4) C(30) 0.070(6) 0.052(5) 0.083(6) -0.001(4) -0.006(5) -0.005(5) C(31) 0.106(8) 0.080(7) 0.140(9) -0.048(7) 0.013(8) 0.012(8) C(32) 0.18(1) 0.130(9) 0.26(1) -0.069(9) 0.01(1) 0.029(10) C(33) 0.076(6) 0.051(5) 0.068(5) 0.016(4) 0.001(5) -0.006(5) C(34) 0.050(5) 0.085(7) 0.098(7) 0.012(5) -0.009(5) 0.018(6) C(35) 0.073(7) 0.13(1) 0.134(10) 0.025(7) 0.012(7) 0.020(9) C(36) 0.067(6) 0.29(2) 0.18(1) 0.026(8) 0.002(7) 0.05(1) #--------------------------------------------------------------------------- #-- _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) 1.215(7) . . yes O(2) C(8) 1.459(6) . . yes O(2) C(9) 1.398(6) . . yes N(1) C(11) 1.383(6) . . yes N(1) C(29) 1.470(8) . . yes N(1) C(33) 1.437(8) . . yes C(1) C(2) 1.475(8) . . yes C(1) C(16) 1.484(8) . . yes C(2) C(3) 1.401(9) . . yes C(2) C(7) 1.390(8) . . yes C(3) C(4) 1.35(1) . . yes C(4) C(5) 1.37(1) . . yes C(5) C(6) 1.400(10) . . yes C(6) C(7) 1.373(8) . . yes C(7) C(8) 1.519(8) . . yes C(8) C(16) 1.511(7) . . yes C(8) C(17) 1.518(7) . . yes C(9) C(10) 1.364(7) . . yes C(9) C(14) 1.393(7) . . yes C(10) C(11) 1.406(8) . . yes C(11) C(12) 1.413(8) . . yes C(12) C(13) 1.372(8) . . yes C(13) C(14) 1.397(8) . . yes C(14) C(15) 1.453(7) . . yes C(15) C(16) 1.347(7) . . yes C(15) C(23) 1.497(7) . . yes C(17) C(18) 1.384(8) . . yes C(17) C(22) 1.378(8) . . yes C(18) C(19) 1.382(9) . . yes C(19) C(20) 1.378(9) . . yes C(20) C(21) 1.369(9) . . yes C(21) C(22) 1.359(9) . . yes C(23) C(24) 1.365(9) . . yes C(23) C(28) 1.385(9) . . yes C(24) C(25) 1.385(9) . . yes C(25) C(26) 1.37(1) . . yes C(26) C(27) 1.34(1) . . yes C(27) C(28) 1.40(1) . . yes C(29) C(30) 1.524(9) . . yes C(30) C(31) 1.51(1) . . yes C(31) C(32) 1.46(1) . . yes C(33) C(34) 1.517(10) . . yes C(34) C(35) 1.50(1) . . yes C(35) C(36) 1.47(1) . . 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(2) C(9) 112.3(4) . . . yes C(11) N(1) C(29) 121.2(6) . . . yes C(11) N(1) C(33) 121.9(6) . . . yes C(29) N(1) C(33) 116.4(6) . . . yes O(1) C(1) C(2) 126.1(6) . . . yes O(1) C(1) C(16) 129.0(6) . . . yes C(2) C(1) C(16) 104.8(6) . . . yes C(1) C(2) C(3) 128.8(7) . . . yes C(1) C(2) C(7) 111.5(6) . . . yes C(3) C(2) C(7) 119.6(7) . . . yes C(2) C(3) C(4) 118.0(8) . . . yes C(3) C(4) C(5) 123.0(8) . . . yes C(4) C(5) C(6) 119.7(8) . . . yes C(5) C(6) C(7) 117.9(7) . . . yes C(2) C(7) C(6) 121.7(6) . . . yes C(2) C(7) C(8) 110.0(6) . . . yes C(6) C(7) C(8) 128.2(6) . . . yes O(2) C(8) C(7) 109.1(5) . . . yes O(2) C(8) C(16) 109.1(5) . . . yes O(2) C(8) C(17) 110.0(5) . . . yes C(7) C(8) C(16) 103.0(5) . . . yes C(7) C(8) C(17) 112.0(5) . . . yes C(16) C(8) C(17) 113.4(5) . . . yes O(2) C(9) C(10) 116.1(5) . . . yes O(2) C(9) C(14) 120.2(6) . . . yes C(10) C(9) C(14) 123.5(6) . . . yes C(9) C(10) C(11) 120.1(6) . . . yes N(1) C(11) C(10) 121.2(6) . . . yes N(1) C(11) C(12) 121.1(6) . . . yes C(10) C(11) C(12) 117.7(6) . . . yes C(11) C(12) C(13) 119.6(7) . . . yes C(12) C(13) C(14) 123.3(6) . . . yes C(9) C(14) C(13) 115.3(6) . . . yes C(9) C(14) C(15) 120.2(6) . . . yes C(13) C(14) C(15) 124.3(6) . . . yes C(14) C(15) C(16) 115.9(6) . . . yes C(14) C(15) C(23) 119.2(6) . . . yes C(16) C(15) C(23) 124.7(6) . . . yes C(1) C(16) C(8) 109.9(6) . . . yes C(1) C(16) C(15) 129.2(6) . . . yes C(8) C(16) C(15) 119.6(6) . . . yes C(8) C(17) C(18) 121.9(6) . . . yes C(8) C(17) C(22) 119.8(6) . . . yes C(18) C(17) C(22) 118.3(7) . . . yes C(17) C(18) C(19) 119.9(7) . . . yes C(18) C(19) C(20) 120.9(8) . . . yes C(19) C(20) C(21) 118.7(8) . . . yes C(20) C(21) C(22) 120.7(8) . . . yes C(17) C(22) C(21) 121.5(8) . . . yes C(15) C(23) C(24) 122.0(7) . . . yes C(15) C(23) C(28) 119.1(7) . . . yes C(24) C(23) C(28) 118.9(7) . . . yes C(23) C(24) C(25) 121.1(9) . . . yes C(24) C(25) C(26) 119.8(9) . . . yes C(25) C(26) C(27) 120.0(9) . . . yes C(26) C(27) C(28) 121.2(10) . . . yes C(23) C(28) C(27) 118.9(9) . . . yes N(1) C(29) C(30) 115.5(6) . . . yes C(29) C(30) C(31) 109.9(8) . . . yes C(30) C(31) C(32) 112.2(10) . . . yes N(1) C(33) C(34) 114.6(7) . . . yes C(33) C(34) C(35) 113.5(8) . . . yes C(34) C(35) C(36) 113.5(10) . . . yes #--------------------------------------------------------------------------- #-- #===============================================END data_3c _database_code_depnum_ccdc_archive 'CCDC 605730' _audit_creation_date 'Thu Dec 22 11:15:08 2005' _audit_creation_method 'by teXsan' _audit_update_record ? #--------------------------------------------------------------------------- #-- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------------- #-- _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 519.70 _chemical_formula_analytical ? _chemical_formula_sum ' C34 H33 N O2 S ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_melting_point ? #--------------------------------------------------------------------------- #-- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.009(2) _cell_length_b 13.949(5) _cell_length_c 9.752(2) _cell_angle_alpha 97.99(2) _cell_angle_beta 101.46(2) _cell_angle_gamma 72.82(2) _cell_volume 1397.1(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 17.0 _cell_measurement_temperature 296.2 #--------------------------------------------------------------------------- #-- _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.400 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.147 _exptl_crystal_F_000 552.00 _exptl_absorpt_correction_T_min 0.869 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #--------------------------------------------------------------------------- #-- _diffrn_special_details ; ? ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 6801 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0000 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.20 _reflns_number_total 6426 _reflns_number_gt 2675 _reflns_threshold_expression F^2^>2.0\s(F^2^) _diffrn_orient_matrix_UB_11 -0.066480 _diffrn_orient_matrix_UB_12 -0.001750 _diffrn_orient_matrix_UB_13 -0.085950 _diffrn_orient_matrix_UB_21 -0.069830 _diffrn_orient_matrix_UB_22 0.029430 _diffrn_orient_matrix_UB_23 0.057900 _diffrn_orient_matrix_UB_31 -0.000930 _diffrn_orient_matrix_UB_32 0.069310 _diffrn_orient_matrix_UB_33 -0.016980 #--------------------------------------------------------------------------- #-- _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 6426 _refine_ls_number_parameters 432 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.04000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_R_factor_all 0.15428 _refine_ls_R_factor_gt 0.08277 _refine_ls_wR_factor_ref 0.22675 _refine_ls_wR_factor_gt 0.20434 _refine_ls_goodness_of_fit_ref 1.779 _refine_ls_shift/su_max 0.3454 _refine_diff_density_max 0.54 _refine_diff_density_min -0.41 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H H 0.000 0.000 'International Tables Vol C Table 6.1.1.2' N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' S S 0.125 0.123 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' #--------------------------------------------------------------------------- #-- 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_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S(1) S 0.1482(1) 0.3387(1) 0.0264(2) 0.1067(5) Uani 1.00 d . . . O(1) O 0.3937(3) 0.5342(2) 0.1492(3) 0.0801(8) Uani 1.00 d . . . O(2) O 0.5970(2) 0.2274(1) 0.3433(2) 0.0507(6) Uani 1.00 d . . . N(1) N 0.5137(3) -0.0922(2) 0.2795(3) 0.0573(8) Uani 1.00 d . . . C(1) C 0.4743(3) 0.4652(2) 0.2084(3) 0.0558(9) Uani 1.00 d . . . C(2) C 0.5721(3) 0.4773(2) 0.3334(3) 0.0539(9) Uani 1.00 d . . . C(3) C 0.5852(4) 0.5664(3) 0.4120(4) 0.064(1) Uani 1.00 d . . . C(4) C 0.6799(5) 0.5582(3) 0.5279(4) 0.076(1) Uani 1.00 d . . . C(5) C 0.7606(4) 0.4655(3) 0.5656(4) 0.079(1) Uani 1.00 d . . . C(6) C 0.7483(4) 0.3775(3) 0.4860(4) 0.067(1) Uani 1.00 d . . . C(7) C 0.6522(3) 0.3849(2) 0.3702(3) 0.0526(9) Uani 1.00 d . . . C(8) C 0.6187(3) 0.3012(2) 0.2667(3) 0.0488(8) Uani 1.00 d . . . C(9) C 0.5292(3) 0.1654(2) 0.2607(3) 0.0458(8) Uani 1.00 d . . . C(10) C 0.5535(3) 0.0706(2) 0.3047(4) 0.0498(9) Uani 1.00 d . . . C(11) C 0.4877(3) 0.0022(2) 0.2353(3) 0.0491(8) Uani 1.00 d . . . C(12) C 0.3951(3) 0.0349(2) 0.1160(4) 0.0526(9) Uani 1.00 d . . . C(13) C 0.3729(3) 0.1291(2) 0.0734(3) 0.0492(9) Uani 1.00 d . . . C(14) C 0.4378(3) 0.1983(2) 0.1439(3) 0.0453(8) Uani 1.00 d . . . C(15) C 0.4100(3) 0.3023(2) 0.1110(3) 0.0466(8) Uani 1.00 d . . . C(16) C 0.4955(3) 0.3552(2) 0.1769(3) 0.0474(8) Uani 1.00 d . . . C(17) C 0.7283(3) 0.2513(2) 0.1832(3) 0.0504(9) Uani 1.00 d . . . C(18) C 0.8120(4) 0.1559(3) 0.2071(4) 0.067(1) Uani 1.00 d . . . C(19) C 0.9148(4) 0.1173(3) 0.1370(5) 0.083(1) Uani 1.00 d . . . C(20) C 0.9384(4) 0.1727(4) 0.0442(5) 0.083(1) Uani 1.00 d . . . C(21) C 0.8561(4) 0.2651(3) 0.0182(5) 0.072(1) Uani 1.00 d . . . C(22) C 0.7520(4) 0.3043(3) 0.0857(4) 0.060(1) Uani 1.00 d . . . C(23) C 0.2930(3) 0.3491(2) 0.0153(3) 0.0523(8) Uani 1.00 d . . . C(24) C 0.2894(2) 0.4126(2) -0.1047(2) 0.0269(6) Uani 1.00 d . . . C(25) C 0.1546(4) 0.4406(3) -0.1628(4) 0.086(1) Uani 1.00 d . . . C(26) C 0.0729(4) 0.4068(3) -0.1079(5) 0.099(2) Uani 1.00 d . . . C(27) C 0.4490(4) -0.1681(3) 0.2100(4) 0.057(1) Uani 1.00 d . . . C(28) C 0.3468(4) -0.1781(3) 0.2853(4) 0.059(1) Uani 1.00 d . . . C(29) C 0.2310(4) -0.0863(3) 0.2876(5) 0.066(1) Uani 1.00 d . . . C(30) C 0.1314(4) -0.1006(3) 0.3640(4) 0.091(2) Uani 1.00 d . . . C(31) C 0.6159(4) -0.1249(3) 0.3982(4) 0.069(1) Uani 1.00 d . . . C(32) C 0.7499(5) -0.1615(4) 0.3589(6) 0.092(2) Uani 1.00 d . . . C(33) C 0.8626(6) -0.1869(7) 0.4733(8) 0.185(3) Uani 1.00 d . . . C(34) C 0.8693(9) -0.2569(7) 0.5717(9) 0.214(4) Uani 1.00 d . . . H(1) H 0.521(3) 0.630(2) 0.377(3) 0.056(9) Uiso 1.00 calc . . . H(2) H 0.688(4) 0.609(3) 0.584(4) 0.09(1) Uiso 1.00 calc . . . H(3) H 0.832(3) 0.461(2) 0.646(3) 0.060(9) Uiso 1.00 calc . . . H(4) H 0.814(3) 0.307(3) 0.496(3) 0.08(1) Uiso 1.00 calc . . . H(5) H 0.617(3) 0.055(2) 0.370(3) 0.034(8) Uiso 1.00 calc . . . H(6) H 0.354(3) -0.003(2) 0.060(3) 0.052(10) Uiso 1.00 calc . . . H(7) H 0.318(3) 0.142(2) -0.009(3) 0.050(9) Uiso 1.00 calc . . . H(8) H 0.801(3) 0.118(2) 0.281(3) 0.07(1) Uiso 1.00 calc . . . H(9) H 0.955(4) 0.052(3) 0.133(4) 0.10(1) Uiso 1.00 calc . . . H(10) H 1.012(5) 0.136(4) -0.003(5) 0.14(2) Uiso 1.00 calc . . . H(11) H 0.851(3) 0.298(3) -0.053(4) 0.08(1) Uiso 1.00 calc . . . H(12) H 0.691(3) 0.365(3) 0.064(3) 0.08(1) Uiso 1.00 calc . . . H(13) H 0.3584 0.4287 -0.1326 0.0323 Uiso 1.00 calc . . . H(14) H 0.1231 0.4821 -0.2388 0.1027 Uiso 1.00 calc . . . H(15) H -0.0169 0.4205 -0.1421 0.1193 Uiso 1.00 calc . . . H(16) H 0.523(3) -0.228(2) 0.202(3) 0.048(8) Uiso 1.00 calc . . . H(17) H 0.418(2) -0.153(2) 0.127(3) 0.028(7) Uiso 1.00 calc . . . H(18) H 0.387(2) -0.185(2) 0.376(3) 0.032(7) Uiso 1.00 calc . . . H(19) H 0.312(3) -0.242(2) 0.230(3) 0.067(9) Uiso 1.00 calc . . . H(20) H 0.264(3) -0.037(3) 0.335(3) 0.07(1) Uiso 1.00 calc . . . H(21) H 0.180(3) -0.075(2) 0.186(4) 0.08(1) Uiso 1.00 calc . . . H(22) H 0.0612 -0.0414 0.3634 0.1096 Uiso 1.00 calc . . . H(23) H 0.1010 -0.1560 0.3184 0.1096 Uiso 1.00 calc . . . H(24) H 0.1693 -0.1138 0.4584 0.1096 Uiso 1.00 calc . . . H(25) H 0.599(3) -0.060(3) 0.482(4) 0.10(1) Uiso 1.00 calc . . . H(26) H 0.592(3) -0.182(3) 0.428(3) 0.08(1) Uiso 1.00 calc . . . H(27) H 0.763(4) -0.096(3) 0.318(4) 0.11(1) Uiso 1.00 calc . . . H(28) H 0.749(4) -0.207(3) 0.288(4) 0.08(1) Uiso 1.00 calc . . . H(29) H 0.8647 -0.1243 0.5285 0.2277 Uiso 1.00 calc . . . H(30) H 0.9372 -0.2103 0.4306 0.2277 Uiso 1.00 calc . . . H(31) H 0.9472 -0.2651 0.6387 0.2635 Uiso 1.00 calc . . . H(32) H 0.8715 -0.3224 0.5212 0.2635 Uiso 1.00 calc . . . H(33) H 0.7978 -0.2366 0.6184 0.2635 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 S(1) 0.0697(7) 0.1068(10) 0.142(1) -0.0150(6) 0.0042(7) 0.0437(8) O(1) 0.107(2) 0.040(1) 0.079(2) -0.007(1) -0.009(1) 0.020(1) O(2) 0.066(1) 0.041(1) 0.046(1) -0.0173(10) 0.002(1) 0.0153(9) N(1) 0.073(2) 0.039(1) 0.063(2) -0.017(1) 0.006(1) 0.019(1) C(1) 0.074(2) 0.041(1) 0.055(2) -0.015(1) 0.012(1) 0.013(1) C(2) 0.072(2) 0.046(1) 0.047(2) -0.017(1) 0.014(1) 0.010(1) C(3) 0.092(3) 0.047(2) 0.062(2) -0.027(2) 0.023(2) 0.004(1) C(4) 0.113(3) 0.062(2) 0.064(2) -0.047(2) 0.008(2) 0.000(2) C(5) 0.098(3) 0.073(2) 0.068(3) -0.043(2) -0.009(2) 0.006(2) C(6) 0.073(2) 0.061(2) 0.064(2) -0.022(2) -0.005(2) 0.013(2) C(7) 0.066(2) 0.046(2) 0.051(2) -0.021(1) 0.010(1) 0.011(1) C(8) 0.059(2) 0.040(2) 0.049(2) -0.014(1) 0.003(1) 0.017(1) C(9) 0.052(2) 0.041(1) 0.048(2) -0.014(1) 0.009(1) 0.010(1) C(10) 0.055(2) 0.046(2) 0.049(2) -0.012(1) 0.001(2) 0.020(1) C(11) 0.058(2) 0.038(1) 0.052(2) -0.008(1) 0.013(1) 0.012(1) C(12) 0.057(2) 0.045(2) 0.056(2) -0.016(2) 0.004(1) 0.007(2) C(13) 0.053(2) 0.046(2) 0.046(2) -0.010(1) 0.000(2) 0.014(1) C(14) 0.050(2) 0.041(1) 0.048(2) -0.010(1) 0.012(1) 0.014(1) C(15) 0.052(2) 0.039(1) 0.047(2) -0.002(1) 0.014(1) 0.012(1) C(16) 0.058(2) 0.039(1) 0.047(2) -0.012(1) 0.008(1) 0.015(1) C(17) 0.048(2) 0.046(2) 0.055(2) -0.012(1) 0.002(1) 0.008(1) C(18) 0.065(2) 0.059(2) 0.073(2) -0.003(2) 0.006(2) 0.025(2) C(19) 0.068(3) 0.068(3) 0.099(3) 0.008(2) 0.016(2) 0.014(2) C(20) 0.063(3) 0.094(3) 0.090(3) -0.016(2) 0.022(2) 0.002(2) C(21) 0.071(2) 0.085(2) 0.074(3) -0.032(2) 0.022(2) 0.012(2) C(22) 0.061(2) 0.057(2) 0.067(2) -0.021(2) 0.010(2) 0.016(2) C(23) 0.054(2) 0.046(2) 0.053(2) -0.007(1) 0.006(1) 0.012(1) C(24) 0.032(1) 0.013(1) 0.030(1) -0.0025(10) -0.001(1) 0.0036(9) C(25) 0.090(2) 0.062(2) 0.086(3) 0.001(2) -0.011(2) 0.025(2) C(26) 0.053(2) 0.091(3) 0.130(4) 0.002(2) -0.020(2) 0.029(2) C(27) 0.078(3) 0.038(2) 0.057(2) -0.014(2) 0.009(2) 0.011(2) C(28) 0.073(2) 0.047(2) 0.060(2) -0.021(1) 0.000(2) 0.017(2) C(29) 0.072(2) 0.053(2) 0.074(3) -0.018(2) 0.005(2) 0.014(2) C(30) 0.080(3) 0.114(3) 0.091(3) -0.023(3) 0.028(2) 0.033(3) C(31) 0.089(2) 0.050(2) 0.068(2) -0.021(2) 0.000(2) 0.025(2) C(32) 0.081(2) 0.062(3) 0.122(4) -0.008(2) 0.009(2) 0.008(3) C(33) 0.107(5) 0.262(9) 0.154(6) -0.007(5) -0.022(4) 0.067(5) C(34) 0.225(9) 0.255(10) 0.198(8) -0.130(8) -0.026(7) 0.079(6) #--------------------------------------------------------------------------- #-- _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 S(1) C(23) 1.668(4) . . yes S(1) C(26) 1.660(6) . . yes O(1) C(1) 1.222(5) . . yes O(2) C(8) 1.450(4) . . yes O(2) C(9) 1.380(4) . . yes N(1) C(11) 1.373(5) . . yes N(1) C(27) 1.464(6) . . yes N(1) C(31) 1.463(6) . . yes C(1) C(2) 1.484(6) . . yes C(1) C(16) 1.479(5) . . yes C(2) C(3) 1.396(6) . . yes C(2) C(7) 1.378(5) . . yes C(3) C(4) 1.370(7) . . yes C(4) C(5) 1.385(8) . . yes C(5) C(6) 1.386(7) . . yes C(6) C(7) 1.378(6) . . yes C(7) C(8) 1.516(6) . . yes C(8) C(16) 1.511(5) . . yes C(8) C(17) 1.530(6) . . yes C(9) C(10) 1.380(5) . . yes C(9) C(14) 1.392(5) . . yes C(10) C(11) 1.389(6) . . yes C(11) C(12) 1.416(6) . . yes C(12) C(13) 1.371(5) . . yes C(13) C(14) 1.395(6) . . yes C(14) C(15) 1.459(5) . . yes C(15) C(16) 1.372(6) . . yes C(15) C(23) 1.467(5) . . yes C(17) C(18) 1.396(6) . . yes C(17) C(22) 1.388(6) . . yes C(18) C(19) 1.373(7) . . yes C(19) C(20) 1.373(8) . . yes C(20) C(21) 1.363(8) . . yes C(21) C(22) 1.369(7) . . yes C(23) C(24) 1.550(5) . . yes C(24) C(25) 1.435(6) . . yes C(25) C(26) 1.352(8) . . yes C(27) C(28) 1.508(7) . . yes C(28) C(29) 1.519(7) . . yes C(29) C(30) 1.515(7) . . yes C(31) C(32) 1.519(8) . . yes C(32) C(33) 1.486(10) . . yes C(33) C(34) 1.439(8) . . 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(23) S(1) C(26) 93.9(3) . . . yes C(8) O(2) C(9) 113.6(3) . . . yes C(11) N(1) C(27) 124.0(4) . . . yes C(11) N(1) C(31) 120.6(4) . . . yes C(27) N(1) C(31) 115.3(4) . . . yes O(1) C(1) C(2) 125.2(4) . . . yes O(1) C(1) C(16) 129.3(4) . . . yes C(2) C(1) C(16) 105.4(3) . . . yes C(1) C(2) C(3) 127.9(4) . . . yes C(1) C(2) C(7) 110.7(4) . . . yes C(3) C(2) C(7) 121.3(4) . . . yes C(2) C(3) C(4) 117.4(5) . . . yes C(3) C(4) C(5) 121.6(5) . . . yes C(4) C(5) C(6) 120.8(5) . . . yes C(5) C(6) C(7) 118.0(5) . . . yes C(2) C(7) C(6) 120.9(4) . . . yes C(2) C(7) C(8) 110.6(4) . . . yes C(6) C(7) C(8) 128.5(4) . . . yes O(2) C(8) C(7) 109.0(3) . . . yes O(2) C(8) C(16) 111.2(3) . . . yes O(2) C(8) C(17) 110.0(3) . . . yes C(7) C(8) C(16) 103.0(3) . . . yes C(7) C(8) C(17) 110.2(3) . . . yes C(16) C(8) C(17) 113.2(3) . . . yes O(2) C(9) C(10) 115.9(4) . . . yes O(2) C(9) C(14) 121.8(3) . . . yes C(10) C(9) C(14) 122.3(4) . . . yes C(9) C(10) C(11) 122.0(4) . . . yes N(1) C(11) C(10) 121.4(4) . . . yes N(1) C(11) C(12) 122.5(4) . . . yes C(10) C(11) C(12) 116.1(4) . . . yes C(11) C(12) C(13) 121.0(4) . . . yes C(12) C(13) C(14) 122.9(4) . . . yes C(9) C(14) C(13) 115.6(3) . . . yes C(9) C(14) C(15) 119.0(4) . . . yes C(13) C(14) C(15) 125.2(4) . . . yes C(14) C(15) C(16) 117.2(4) . . . yes C(14) C(15) C(23) 121.2(4) . . . yes C(16) C(15) C(23) 121.6(3) . . . yes C(1) C(16) C(8) 109.2(3) . . . yes C(1) C(16) C(15) 129.5(4) . . . yes C(8) C(16) C(15) 119.1(3) . . . yes C(8) C(17) C(18) 122.6(4) . . . yes C(8) C(17) C(22) 119.5(4) . . . yes C(18) C(17) C(22) 117.8(4) . . . yes C(17) C(18) C(19) 120.5(5) . . . yes C(18) C(19) C(20) 120.5(5) . . . yes C(19) C(20) C(21) 119.5(6) . . . yes C(20) C(21) C(22) 120.8(5) . . . yes C(17) C(22) C(21) 120.9(5) . . . yes S(1) C(23) C(15) 122.4(3) . . . yes S(1) C(23) C(24) 113.1(3) . . . yes C(15) C(23) C(24) 124.5(3) . . . yes C(23) C(24) C(25) 101.9(4) . . . yes C(24) C(25) C(26) 119.0(4) . . . yes S(1) C(26) C(25) 112.1(4) . . . yes N(1) C(27) C(28) 113.5(4) . . . yes C(27) C(28) C(29) 114.8(4) . . . yes C(28) C(29) C(30) 112.5(4) . . . yes N(1) C(31) C(32) 113.5(5) . . . yes C(31) C(32) C(33) 118.3(7) . . . yes C(32) C(33) C(34) 120.6(9) . . . yes #--------------------------------------------------------------------------- #-- #===============================================END