# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Prof Katsuhira Yoshida' _publ_contact_author_address ; Department of Material Science Kochi University Akebono-cho Kochi 780-8520 JAPAN ; _publ_contact_author_email kyoshida@cc.kochi-u.ac.jp _publ_section_title ; Heterocyclic quinol-type fluorophores: Synthesis of novel imidazoanthraquinol derivatives and their photophysical properties in benzene and in the crystalline state ; _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 K.Yoshida N.Takato O.Yousuke data_2a _database_code_depnum_ccdc_archive 'CCDC 236773' _audit_creation_date 'Tue Oct 26 23:53:16 2004' _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 411.50 _chemical_formula_analytical ? _chemical_formula_sum ' C26 H25 N3 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 11.111(2) _cell_length_b 16.954(2) _cell_length_c 12.318(2) _cell_angle_alpha 90 _cell_angle_beta 113.97(1) _cell_angle_gamma 90 _cell_volume 2120.3(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.9 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #---------------------------------------------------- _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.450 _exptl_crystal_size_min 0.250 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872.00 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.968 _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 3936 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 0.9987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.9987 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.34 _reflns_number_total 3735 _reflns_number_gt 1866 _reflns_threshold_expression >2sigma(I) _diffrn_orient_matrix_UB_11 -0.00200 _diffrn_orient_matrix_UB_12 -0.04201 _diffrn_orient_matrix_UB_13 -0.05769 _diffrn_orient_matrix_UB_21 -0.09728 _diffrn_orient_matrix_UB_22 0.00726 _diffrn_orient_matrix_UB_23 -0.04347 _diffrn_orient_matrix_UB_31 0.01528 _diffrn_orient_matrix_UB_32 0.04076 _diffrn_orient_matrix_UB_33 -0.05172 #-------------------------------------------------- _refine_special_details ; Refinement F^2^ against All reflections. 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 3735 _refine_ls_number_parameters 341 _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 0.0994 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1457 _refine_ls_goodness_of_fit_ref 1.444 _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 0.49 _refine_diff_density_min -0.62 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.010(2) _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 0.0033 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H H 0.0000 0.0000 'International Tables Vol C Table 6.1.1.2' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O O 0.0106 0.0060 '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 -0.4765(2) -0.1851(1) -1.0081(2) 0.0637(8) Uani 1.00 d . . . O(2) O -0.9889(3) -0.1378(2) -1.0880(3) 0.106(1) Uani 1.00 d . . . N(1) N -0.4107(3) -0.0526(2) -0.8461(3) 0.0542(9) Uani 1.00 d . . . N(2) N -0.4738(3) 0.0639(2) -0.8028(3) 0.0598(9) Uani 1.00 d . . . N(3) N 0.1545(4) 0.1089(3) -0.5320(5) 0.153(2) Uani 1.00 d . . . C(1) C -0.5910(3) -0.1927(2) -0.9814(3) 0.0544(10) Uani 1.00 d . . . C(2) C -0.6983(4) -0.2383(2) -1.0781(3) 0.062(1) Uani 1.00 d . . . C(3) C -0.6643(5) -0.3044(2) -1.1265(4) 0.074(1) Uani 1.00 d . . . C(4) C -0.7602(6) -0.3492(3) -1.2125(4) 0.090(2) Uani 1.00 d . . . C(5) C -0.8906(6) -0.3290(3) -1.2508(4) 0.097(2) Uani 1.00 d . . . C(6) C -0.9260(5) -0.2648(3) -1.2036(4) 0.085(2) Uani 1.00 d . . . C(7) C -0.8308(4) -0.2189(2) -1.1154(3) 0.067(1) Uani 1.00 d . . . C(8) C -0.8718(4) -0.1484(2) -1.0676(3) 0.072(1) Uani 1.00 d . . . C(9) C -0.7681(3) -0.0922(2) -0.9973(3) 0.060(1) Uani 1.00 d . . . C(10) C -0.8061(4) -0.0185(2) -0.9696(4) 0.068(1) Uani 1.00 d . . . C(11) C -0.7170(4) 0.0372(2) -0.9070(4) 0.068(1) Uani 1.00 d . . . C(12) C -0.5839(3) 0.0190(2) -0.8684(3) 0.055(1) Uani 1.00 d . . . C(13) C -0.5465(3) -0.0543(2) -0.8968(3) 0.0504(10) Uani 1.00 d . . . C(14) C -0.6360(3) -0.1120(2) -0.9613(3) 0.0526(10) Uani 1.00 d . . . C(15) C -0.3720(3) 0.0185(2) -0.7913(3) 0.054(1) Uani 1.00 d . . . C(16) C -0.2346(3) 0.0401(2) -0.7244(3) 0.057(1) Uani 1.00 d . . . C(17) C -0.2014(4) 0.1034(2) -0.6452(4) 0.068(1) Uani 1.00 d . . . C(18) C -0.0749(4) 0.1258(3) -0.5820(4) 0.078(1) Uani 1.00 d . . . C(19) C 0.0281(4) 0.0864(3) -0.5943(4) 0.086(2) Uani 1.00 d . . . C(20) C -0.0029(4) 0.0224(3) -0.6720(4) 0.081(1) Uani 1.00 d . . . C(21) C -0.1306(4) -0.0001(2) -0.7341(4) 0.066(1) Uani 1.00 d . . . C(22) C 0.1984(5) 0.1647(4) -0.4178(7) 0.150(3) Uani 1.00 d . . . C(23) C 0.1955(6) 0.2349(4) -0.4699(7) 0.163(3) Uani 1.00 d . . . C(24) C 0.293(1) 0.0509(5) -0.5170(7) 0.204(4) Uani 1.00 d . . . C(25) C 0.2784(7) 0.0929(4) -0.6114(7) 0.163(3) Uani 1.00 d . . . C(26) C -0.5429(4) -0.2394(2) -0.8649(4) 0.065(1) Uani 1.00 d . . . H(1) H -0.500(4) -0.154(2) -1.072(3) 0.09(1) Uiso 1.00 calc . . . H(2) H -0.362(3) -0.089(2) -0.855(3) 0.07(1) Uiso 1.00 calc . . . H(3) H -0.572(3) -0.321(2) -1.100(3) 0.08(1) Uiso 1.00 calc . . . H(4) H -0.732(4) -0.394(2) -1.249(3) 0.09(1) Uiso 1.00 calc . . . H(5) H -0.954(4) -0.358(3) -1.312(4) 0.11(1) Uiso 1.00 calc . . . H(6) H -1.010(4) -0.245(2) -1.221(3) 0.08(1) Uiso 1.00 calc . . . H(7) H -0.900(4) -0.007(2) -1.001(3) 0.09(1) Uiso 1.00 calc . . . H(8) H -0.739(3) 0.088(2) -0.889(3) 0.062(9) Uiso 1.00 calc . . . H(9) H -0.264(3) 0.129(2) -0.636(3) 0.07(1) Uiso 1.00 calc . . . H(10) H -0.063(3) 0.174(2) -0.537(3) 0.07(1) Uiso 1.00 calc . . . H(11) H 0.063(4) -0.007(2) -0.684(3) 0.09(1) Uiso 1.00 calc . . . H(12) H -0.145(3) -0.048(2) -0.781(3) 0.09(1) Uiso 1.00 calc . . . H(13) H 0.1320 0.1579 -0.3853 0.1626 Uiso 1.00 calc . . . H(14) H 0.2792 0.1468 -0.3612 0.1626 Uiso 1.00 calc . . . H(15) H 0.2430 0.2322 -0.5204 0.1881 Uiso 1.00 calc . . . H(16) H 0.2351 0.2736 -0.4112 0.1881 Uiso 1.00 calc . . . H(17) H 0.1069 0.2511 -0.5193 0.1881 Uiso 1.00 calc . . . H(18) H 0.2621 -0.0067 -0.5283 0.1503 Uiso 1.00 calc . . . H(19) H 0.3752 0.0360 -0.5598 0.0520 Uiso 1.00 calc . . . H(20) H 0.3545 0.1228 -0.5962 0.1920 Uiso 1.00 calc . . . H(21) H 0.2045 0.1277 -0.6282 0.1920 Uiso 1.00 calc . . . H(22) H 0.2604 0.0591 -0.6770 0.1920 Uiso 1.00 calc . . . H(23) H -0.615(3) -0.240(2) -0.837(3) 0.07(1) Uiso 1.00 calc . . . H(24) H -0.468(4) -0.213(3) -0.802(4) 0.11(1) Uiso 1.00 calc . . . H(25) H -0.514(4) -0.294(2) -0.879(3) 0.10(1) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(1) 0.059(2) 0.052(1) 0.091(2) 0.001(1) 0.042(1) 0.003(1) O(2) 0.053(2) 0.126(3) 0.138(3) -0.012(2) 0.037(2) -0.008(2) N(1) 0.047(2) 0.045(2) 0.071(2) 0.004(1) 0.025(2) 0.001(1) N(2) 0.058(2) 0.050(2) 0.076(2) 0.000(1) 0.033(2) -0.002(1) N(3) 0.075(3) 0.183(5) 0.188(5) -0.037(3) 0.041(3) -0.127(4) C(1) 0.054(2) 0.050(2) 0.066(2) -0.004(2) 0.031(2) 0.004(2) C(2) 0.075(3) 0.057(2) 0.062(2) -0.015(2) 0.038(2) 0.002(2) C(3) 0.087(3) 0.073(3) 0.068(3) -0.014(2) 0.038(3) -0.004(2) C(4) 0.117(4) 0.079(3) 0.078(3) -0.023(3) 0.046(3) -0.015(3) C(5) 0.120(5) 0.094(4) 0.071(3) -0.044(3) 0.033(3) -0.009(3) C(6) 0.082(3) 0.092(3) 0.079(3) -0.023(3) 0.028(3) 0.004(3) C(7) 0.061(2) 0.072(2) 0.066(2) -0.023(2) 0.025(2) 0.000(2) C(8) 0.056(2) 0.085(3) 0.080(3) -0.008(2) 0.033(2) 0.008(2) C(9) 0.054(2) 0.063(2) 0.065(2) -0.004(2) 0.027(2) 0.006(2) C(10) 0.049(2) 0.075(3) 0.089(3) 0.009(2) 0.036(2) 0.010(2) C(11) 0.067(3) 0.057(2) 0.088(3) 0.012(2) 0.042(2) 0.005(2) C(12) 0.051(2) 0.048(2) 0.072(2) 0.005(2) 0.031(2) 0.006(2) C(13) 0.047(2) 0.050(2) 0.059(2) 0.003(2) 0.027(2) 0.006(2) C(14) 0.045(2) 0.052(2) 0.063(2) 0.002(2) 0.025(2) 0.008(2) C(15) 0.057(2) 0.045(2) 0.063(2) -0.002(2) 0.028(2) 0.000(2) C(16) 0.058(2) 0.050(2) 0.063(2) -0.001(2) 0.026(2) -0.002(2) C(17) 0.068(3) 0.061(2) 0.081(3) 0.002(2) 0.035(2) -0.013(2) C(18) 0.076(3) 0.072(3) 0.085(3) -0.012(2) 0.029(2) -0.031(2) C(19) 0.063(3) 0.092(3) 0.098(3) -0.016(2) 0.029(2) -0.039(3) C(20) 0.061(3) 0.086(3) 0.098(3) -0.001(2) 0.032(2) -0.028(3) C(21) 0.059(2) 0.063(2) 0.074(3) -0.006(2) 0.026(2) -0.015(2) C(22) 0.086(4) 0.151(6) 0.187(7) 0.012(4) 0.029(4) 0.056(5) C(23) 0.110(5) 0.130(5) 0.267(9) 0.010(4) 0.095(5) 0.045(6) C(24) 0.31(1) 0.170(7) 0.129(6) -0.101(8) 0.085(7) -0.007(5) C(25) 0.132(5) 0.163(6) 0.162(7) -0.046(5) 0.026(5) -0.020(6) C(26) 0.073(3) 0.054(2) 0.068(3) 0.001(2) 0.028(2) 0.003(2) #----------------------------------------------------- _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) 1.443(4) 1_555 1_555 yes O(2) C(8) 1.234(4) 1_555 1_555 yes N(1) C(13) 1.379(4) 1_555 1_555 yes N(1) C(15) 1.363(4) 1_555 1_555 yes N(2) C(12) 1.387(4) 1_555 1_555 yes N(2) C(15) 1.327(4) 1_555 1_555 yes N(3) C(19) 1.354(5) 1_555 1_555 yes N(3) C(22) 1.597(8) 1_555 1_555 yes N(3) C(24) 1.78(1) 1_555 1_555 yes C(1) C(2) 1.512(5) 1_555 1_555 yes C(1) C(14) 1.511(4) 1_555 1_555 yes C(1) C(26) 1.532(5) 1_555 1_555 yes C(2) C(3) 1.392(5) 1_555 1_555 yes C(2) C(7) 1.391(5) 1_555 1_555 yes C(3) C(4) 1.384(6) 1_555 1_555 yes C(4) C(5) 1.372(7) 1_555 1_555 yes C(5) C(6) 1.365(7) 1_555 1_555 yes C(6) C(7) 1.405(5) 1_555 1_555 yes C(7) C(8) 1.483(5) 1_555 1_555 yes C(8) C(9) 1.475(5) 1_555 1_555 yes C(9) C(10) 1.405(5) 1_555 1_555 yes C(9) C(14) 1.391(4) 1_555 1_555 yes C(10) C(11) 1.359(5) 1_555 1_555 yes C(11) C(12) 1.392(4) 1_555 1_555 yes C(12) C(13) 1.400(4) 1_555 1_555 yes C(13) C(14) 1.391(4) 1_555 1_555 yes C(15) C(16) 1.457(4) 1_555 1_555 yes C(16) C(17) 1.395(5) 1_555 1_555 yes C(16) C(21) 1.387(4) 1_555 1_555 yes C(17) C(18) 1.356(5) 1_555 1_555 yes C(18) C(19) 1.385(5) 1_555 1_555 yes C(19) C(20) 1.396(5) 1_555 1_555 yes C(20) C(21) 1.365(5) 1_555 1_555 yes C(22) C(23) 1.347(7) 1_555 1_555 yes C(24) C(25) 1.314(9) 1_555 1_555 yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(13) N(1) C(15) 108.0(3) 1_555 1_555 1_555 yes C(12) N(2) C(15) 104.8(3) 1_555 1_555 1_555 yes C(19) N(3) C(22) 122.8(4) 1_555 1_555 1_555 yes C(19) N(3) C(24) 124.1(4) 1_555 1_555 1_555 yes C(22) N(3) C(24) 107.1(4) 1_555 1_555 1_555 yes O(1) C(1) C(2) 110.6(3) 1_555 1_555 1_555 yes O(1) C(1) C(14) 109.7(2) 1_555 1_555 1_555 yes O(1) C(1) C(26) 104.8(3) 1_555 1_555 1_555 yes C(2) C(1) C(14) 112.6(3) 1_555 1_555 1_555 yes C(2) C(1) C(26) 109.7(3) 1_555 1_555 1_555 yes C(14) C(1) C(26) 109.1(3) 1_555 1_555 1_555 yes C(1) C(2) C(3) 119.0(4) 1_555 1_555 1_555 yes C(1) C(2) C(7) 121.9(3) 1_555 1_555 1_555 yes C(3) C(2) C(7) 118.9(4) 1_555 1_555 1_555 yes C(2) C(3) C(4) 120.7(5) 1_555 1_555 1_555 yes C(3) C(4) C(5) 120.3(5) 1_555 1_555 1_555 yes C(4) C(5) C(6) 119.9(5) 1_555 1_555 1_555 yes C(5) C(6) C(7) 120.9(5) 1_555 1_555 1_555 yes C(2) C(7) C(6) 119.2(4) 1_555 1_555 1_555 yes C(2) C(7) C(8) 120.9(3) 1_555 1_555 1_555 yes C(6) C(7) C(8) 119.8(4) 1_555 1_555 1_555 yes O(2) C(8) C(7) 120.4(4) 1_555 1_555 1_555 yes O(2) C(8) C(9) 122.2(4) 1_555 1_555 1_555 yes C(7) C(8) C(9) 117.4(3) 1_555 1_555 1_555 yes C(8) C(9) C(10) 118.5(3) 1_555 1_555 1_555 yes C(8) C(9) C(14) 120.2(3) 1_555 1_555 1_555 yes C(10) C(9) C(14) 121.3(3) 1_555 1_555 1_555 yes C(9) C(10) C(11) 122.3(3) 1_555 1_555 1_555 yes C(10) C(11) C(12) 117.9(4) 1_555 1_555 1_555 yes N(2) C(12) C(11) 129.9(3) 1_555 1_555 1_555 yes N(2) C(12) C(13) 110.6(3) 1_555 1_555 1_555 yes C(11) C(12) C(13) 119.5(3) 1_555 1_555 1_555 yes N(1) C(13) C(12) 104.5(3) 1_555 1_555 1_555 yes N(1) C(13) C(14) 132.1(3) 1_555 1_555 1_555 yes C(12) C(13) C(14) 123.5(3) 1_555 1_555 1_555 yes C(1) C(14) C(9) 122.8(3) 1_555 1_555 1_555 yes C(1) C(14) C(13) 121.5(3) 1_555 1_555 1_555 yes C(9) C(14) C(13) 115.5(3) 1_555 1_555 1_555 yes N(1) C(15) N(2) 112.1(3) 1_555 1_555 1_555 yes N(1) C(15) C(16) 123.4(3) 1_555 1_555 1_555 yes N(2) C(15) C(16) 124.5(3) 1_555 1_555 1_555 yes C(15) C(16) C(17) 120.5(3) 1_555 1_555 1_555 yes C(15) C(16) C(21) 123.1(3) 1_555 1_555 1_555 yes C(17) C(16) C(21) 116.4(3) 1_555 1_555 1_555 yes C(16) C(17) C(18) 122.4(4) 1_555 1_555 1_555 yes C(17) C(18) C(19) 120.8(4) 1_555 1_555 1_555 yes N(3) C(19) C(18) 121.0(4) 1_555 1_555 1_555 yes N(3) C(19) C(20) 121.2(4) 1_555 1_555 1_555 yes C(18) C(19) C(20) 117.8(4) 1_555 1_555 1_555 yes C(19) C(20) C(21) 120.8(4) 1_555 1_555 1_555 yes C(16) C(21) C(20) 121.9(4) 1_555 1_555 1_555 yes N(3) C(22) C(23) 99.4(6) 1_555 1_555 1_555 yes N(3) C(24) C(25) 79.3(7) 1_555 1_555 1_555 yes #----------------------------------------------- #===============================================END data_3a _database_code_depnum_ccdc_archive 'CCDC 236774' _audit_creation_date 'Thu Oct 28 18:42:49 2004' _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 411.50 _chemical_formula_analytical ? _chemical_formula_sum ' C26 H25 N3 O2 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_melting_point ? #---------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z 1/2-x,1/2+y,1/2+z 1/2+x,1/2-y,z _cell_length_a 13.405(6) _cell_length_b 10.911(2) _cell_length_c 14.405(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2106(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.4 _cell_measurement_theta_max 11.9 _cell_measurement_temperature 296.2 #----------------------------------------------- _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.250 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872.00 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_T_min 0.980 _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 2758 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9988 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.03 _reflns_number_total 2516 _reflns_number_gt 1465 _reflns_threshold_expression >2sigma(I) _diffrn_orient_matrix_UB_11 0.002900 _diffrn_orient_matrix_UB_12 -0.048180 _diffrn_orient_matrix_UB_13 -0.059000 _diffrn_orient_matrix_UB_21 0.001970 _diffrn_orient_matrix_UB_22 0.077960 _diffrn_orient_matrix_UB_23 -0.036440 _diffrn_orient_matrix_UB_31 0.074520 _diffrn_orient_matrix_UB_32 -0.000180 _diffrn_orient_matrix_UB_33 0.003250 #------------------------------------------------- _refine_special_details ; Refinement F^2^ against All reflections. 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 2516 _refine_ls_number_parameters 330 _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 0.0736 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_shift/su_max 0.0009 _refine_diff_density_max 0.21 _refine_diff_density_min -0.18 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.011(2) _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 0.0033 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H H 0.0000 0.0000 'International Tables Vol C Table 6.1.1.2' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O O 0.0106 0.0060 '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 0.1921(2) 0.1139(3) 0.877(1) 0.0504(8) Uani 1.00 d . . . O(2) O -0.0391(2) -0.1185(3) 0.621(1) 0.0560(9) Uani 1.00 d . . . N(1) N -0.1961(2) 0.0399(3) 0.665(1) 0.0400(8) Uani 1.00 d . . . N(2) N -0.2603(2) 0.1924(3) 0.751(1) 0.0397(8) Uani 1.00 d . . . N(3) N -0.6411(2) 0.0723(3) 0.484(1) 0.0532(10) Uani 1.00 d . . . C(1) C 0.0126(3) -0.0704(3) 0.681(1) 0.0419(9) Uani 1.00 d . . . C(2) C 0.1212(3) -0.0976(4) 0.690(1) 0.0443(10) Uani 1.00 d . . . C(3) C 0.1664(3) -0.1679(4) 0.621(1) 0.055(1) Uani 1.00 d . . . C(4) C 0.2682(3) -0.1884(5) 0.624(1) 0.067(1) Uani 1.00 d . . . C(5) C 0.3238(3) -0.1401(5) 0.696(1) 0.069(2) Uani 1.00 d . . . C(6) C 0.2788(3) -0.0730(5) 0.764(1) 0.061(1) Uani 1.00 d . . . C(7) C 0.1765(3) -0.0487(4) 0.763(1) 0.0440(10) Uani 1.00 d . . . C(8) C 0.1276(3) 0.0189(4) 0.844(1) 0.0429(10) Uani 1.00 d . . . C(9) C 0.0257(3) 0.0713(3) 0.818(1) 0.0373(9) Uani 1.00 d . . . C(10) C -0.0156(3) 0.1633(4) 0.873(1) 0.0432(10) Uani 1.00 d . . . C(11) C -0.1100(3) 0.2116(4) 0.858(1) 0.0411(10) Uani 1.00 d . . . C(12) C -0.1646(2) 0.1635(4) 0.784(1) 0.0370(9) Uani 1.00 d . . . C(13) C -0.1245(3) 0.0687(4) 0.730(1) 0.0364(9) Uani 1.00 d . . . C(14) C -0.0279(2) 0.0216(3) 0.745(1) 0.0373(9) Uani 1.00 d . . . C(15) C -0.2764(3) 0.1165(4) 0.681(1) 0.0392(9) Uani 1.00 d . . . C(16) C -0.3686(3) 0.1063(4) 0.627(1) 0.0402(9) Uani 1.00 d . . . C(17) C -0.4545(3) 0.1654(4) 0.658(1) 0.046(1) Uani 1.00 d . . . C(18) C -0.5435(3) 0.1531(4) 0.611(1) 0.049(1) Uani 1.00 d . . . C(19) C -0.5518(3) 0.0833(4) 0.530(1) 0.0437(10) Uani 1.00 d . . . C(20) C -0.4641(3) 0.0246(4) 0.500(1) 0.055(1) Uani 1.00 d . . . C(21) C -0.3762(3) 0.0358(4) 0.548(1) 0.050(1) Uani 1.00 d . . . C(22) C -0.7292(3) 0.1343(4) 0.520(1) 0.056(1) Uani 1.00 d . . . C(23) C -0.8241(3) 0.1207(5) 0.467(1) 0.085(2) Uani 1.00 d . . . C(24) C -0.6406(3) 0.0213(4) 0.390(1) 0.061(1) Uani 1.00 d . . . C(25) C -0.6011(5) 0.1080(6) 0.318(1) 0.087(2) Uani 1.00 d . . . C(26) C 0.1135(3) -0.0687(4) 0.925(1) 0.053(1) Uani 1.00 d . . . H(1) H 0.195(4) 0.176(5) 0.822(4) 0.096(8) Uiso 1.00 calc . . . H(2) H -0.194(3) -0.020(4) 0.624(3) 0.065(9) Uiso 1.00 calc . . . H(3) H 0.126(3) -0.195(5) 0.571(4) 0.073(9) Uiso 1.00 calc . . . H(4) H 0.298(3) -0.234(4) 0.576(3) 0.050(9) Uiso 1.00 calc . . . H(5) H 0.399(4) -0.157(5) 0.697(4) 0.100(8) Uiso 1.00 calc . . . H(6) H 0.317(3) -0.038(3) 0.809(3) 0.042(9) Uiso 1.00 calc . . . H(7) H 0.024(2) 0.191(3) 0.929(3) 0.037(8) Uiso 1.00 calc . . . H(8) H -0.137(2) 0.283(3) 0.896(3) 0.044(9) Uiso 1.00 calc . . . H(9) H -0.455(3) 0.221(3) 0.717(3) 0.046(9) Uiso 1.00 calc . . . H(10) H -0.597(3) 0.191(4) 0.632(3) 0.038(9) Uiso 1.00 calc . . . H(11) H -0.467(3) -0.024(4) 0.447(3) 0.056(9) Uiso 1.00 calc . . . H(12) H -0.318(3) -0.009(3) 0.520(3) 0.038(9) Uiso 1.00 calc . . . H(13) H -0.7145 0.2196 0.5226 0.0671 Uiso 1.00 calc . . . H(14) H -0.7410 0.1041 0.5804 0.0671 Uiso 1.00 calc . . . H(15) H -0.8770 0.1638 0.4945 0.0994 Uiso 1.00 calc . . . H(16) H -0.8421 0.0354 0.4615 0.0994 Uiso 1.00 calc . . . H(17) H -0.8156 0.1509 0.4037 0.0994 Uiso 1.00 calc . . . H(18) H -0.5996 -0.0502 0.3879 0.0721 Uiso 1.00 calc . . . H(19) H -0.7067 -0.0007 0.3719 0.0721 Uiso 1.00 calc . . . H(20) H -0.6422 0.1787 0.3161 0.1007 Uiso 1.00 calc . . . H(21) H -0.6029 0.0690 0.2581 0.1007 Uiso 1.00 calc . . . H(22) H -0.5351 0.1294 0.3323 0.1007 Uiso 1.00 calc . . . H(23) H 0.0844 -0.0254 0.9751 0.0635 Uiso 1.00 calc . . . H(24) H 0.0709 -0.1338 0.9066 0.0635 Uiso 1.00 calc . . . H(25) H 0.1764 -0.1004 0.9429 0.0635 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) 0.036(1) 0.058(2) 0.057(2) -0.008(1) -0.013(1) 0.001(2) O(2) 0.043(2) 0.067(2) 0.058(2) 0.004(1) -0.010(1) -0.019(2) N(1) 0.032(1) 0.049(2) 0.039(2) 0.001(1) -0.007(1) -0.005(2) N(2) 0.032(1) 0.048(2) 0.039(2) 0.000(1) -0.003(1) 0.005(1) N(3) 0.033(1) 0.069(2) 0.059(2) 0.006(2) -0.008(1) -0.018(2) C(1) 0.037(2) 0.045(2) 0.044(2) 0.001(1) 0.001(1) 0.002(2) C(2) 0.037(2) 0.051(2) 0.046(2) 0.005(2) -0.001(1) 0.008(2) C(3) 0.052(2) 0.066(3) 0.048(2) 0.017(2) -0.002(2) -0.001(2) C(4) 0.051(2) 0.085(4) 0.066(3) 0.024(2) 0.009(2) -0.002(3) C(5) 0.040(2) 0.085(4) 0.083(3) 0.019(2) 0.000(2) -0.002(2) C(6) 0.036(2) 0.077(3) 0.070(3) 0.005(2) -0.013(2) 0.002(2) C(7) 0.035(2) 0.049(2) 0.048(2) 0.003(2) -0.002(1) 0.010(2) C(8) 0.031(2) 0.053(2) 0.045(2) -0.002(1) -0.008(1) 0.006(1) C(9) 0.032(2) 0.045(2) 0.035(2) -0.004(1) -0.003(1) 0.007(1) C(10) 0.037(2) 0.050(2) 0.042(2) -0.005(2) -0.007(2) -0.001(2) C(11) 0.036(2) 0.048(2) 0.039(2) -0.001(2) 0.001(1) -0.001(2) C(12) 0.028(1) 0.043(2) 0.040(2) -0.001(1) 0.002(1) 0.002(1) C(13) 0.031(2) 0.045(2) 0.034(2) -0.004(1) 0.000(1) 0.003(1) C(14) 0.032(2) 0.043(2) 0.037(2) -0.004(1) -0.001(1) 0.004(2) C(15) 0.034(2) 0.049(2) 0.035(2) 0.002(1) -0.003(1) 0.007(1) C(16) 0.032(2) 0.046(2) 0.042(2) 0.000(1) -0.002(1) 0.003(2) C(17) 0.036(2) 0.054(2) 0.048(2) 0.006(2) -0.005(2) -0.009(2) C(18) 0.034(2) 0.062(3) 0.053(2) 0.010(2) -0.005(2) -0.016(2) C(19) 0.037(2) 0.047(2) 0.046(2) -0.003(2) -0.006(1) -0.003(2) C(20) 0.042(2) 0.069(3) 0.053(3) 0.007(2) -0.008(2) -0.022(2) C(21) 0.038(2) 0.062(3) 0.049(2) 0.005(2) 0.000(2) -0.014(2) C(22) 0.034(2) 0.058(3) 0.076(3) 0.003(2) -0.004(2) -0.009(2) C(23) 0.044(2) 0.105(4) 0.107(4) 0.012(3) -0.026(3) -0.030(4) C(24) 0.053(2) 0.059(3) 0.070(2) 0.002(2) -0.019(2) -0.030(2) C(25) 0.111(5) 0.093(4) 0.057(3) -0.005(3) -0.010(3) -0.013(3) C(26) 0.055(2) 0.062(3) 0.042(2) 0.001(2) -0.008(2) 0.012(2) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(8) 1.432(5) 1_555 1_555 yes O(2) C(1) 1.225(5) 1_555 1_555 yes N(1) C(13) 1.378(4) 1_555 1_555 yes N(1) C(15) 1.382(5) 1_555 1_555 yes N(2) C(12) 1.402(4) 1_555 1_555 yes N(2) C(15) 1.326(5) 1_555 1_555 yes N(3) C(19) 1.378(5) 1_555 1_555 yes N(3) C(22) 1.459(5) 1_555 1_555 yes N(3) C(24) 1.464(6) 1_555 1_555 yes C(1) C(2) 1.491(5) 1_555 1_555 yes C(1) C(14) 1.461(5) 1_555 1_555 yes C(2) C(3) 1.394(6) 1_555 1_555 yes C(2) C(7) 1.394(6) 1_555 1_555 yes C(3) C(4) 1.385(6) 1_555 1_555 yes C(4) C(5) 1.385(8) 1_555 1_555 yes C(5) C(6) 1.357(7) 1_555 1_555 yes C(6) C(7) 1.396(6) 1_555 1_555 yes C(7) C(8) 1.524(6) 1_555 1_555 yes C(8) C(9) 1.525(5) 1_555 1_555 yes C(8) C(26) 1.530(5) 1_555 1_555 yes C(9) C(10) 1.395(5) 1_555 1_555 yes C(9) C(14) 1.392(5) 1_555 1_555 yes C(10) C(11) 1.390(5) 1_555 1_555 yes C(11) C(12) 1.395(5) 1_555 1_555 yes C(12) C(13) 1.397(5) 1_555 1_555 yes C(13) C(14) 1.408(5) 1_555 1_555 yes C(15) C(16) 1.460(5) 1_555 1_555 yes C(16) C(17) 1.390(5) 1_555 1_555 yes C(16) C(21) 1.387(6) 1_555 1_555 yes C(17) C(18) 1.378(5) 1_555 1_555 yes C(18) C(19) 1.391(6) 1_555 1_555 yes C(19) C(20) 1.408(6) 1_555 1_555 yes C(20) C(21) 1.369(6) 1_555 1_555 yes C(22) C(23) 1.491(6) 1_555 1_555 yes C(24) C(25) 1.502(8) 1_555 1_555 yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(13) N(1) C(15) 107.0(3) 1_555 1_555 1_555 yes C(12) N(2) C(15) 105.3(3) 1_555 1_555 1_555 yes C(19) N(3) C(22) 119.2(3) 1_555 1_555 1_555 yes C(19) N(3) C(24) 118.7(3) 1_555 1_555 1_555 yes C(22) N(3) C(24) 120.9(3) 1_555 1_555 1_555 yes O(2) C(1) C(2) 121.7(4) 1_555 1_555 1_555 yes O(2) C(1) C(14) 121.5(3) 1_555 1_555 1_555 yes C(2) C(1) C(14) 116.7(3) 1_555 1_555 1_555 yes C(1) C(2) C(3) 118.4(4) 1_555 1_555 1_555 yes C(1) C(2) C(7) 120.3(4) 1_555 1_555 1_555 yes C(3) C(2) C(7) 121.2(4) 1_555 1_555 1_555 yes C(2) C(3) C(4) 119.6(5) 1_555 1_555 1_555 yes C(3) C(4) C(5) 119.6(5) 1_555 1_555 1_555 yes C(4) C(5) C(6) 120.3(5) 1_555 1_555 1_555 yes C(5) C(6) C(7) 122.3(5) 1_555 1_555 1_555 yes C(2) C(7) C(6) 117.1(4) 1_555 1_555 1_555 yes C(2) C(7) C(8) 122.1(3) 1_555 1_555 1_555 yes C(6) C(7) C(8) 120.6(4) 1_555 1_555 1_555 yes O(1) C(8) C(7) 110.3(3) 1_555 1_555 1_555 yes O(1) C(8) C(9) 110.4(3) 1_555 1_555 1_555 yes O(1) C(8) C(26) 105.5(3) 1_555 1_555 1_555 yes C(7) C(8) C(9) 112.7(3) 1_555 1_555 1_555 yes C(7) C(8) C(26) 109.7(3) 1_555 1_555 1_555 yes C(9) C(8) C(26) 107.9(3) 1_555 1_555 1_555 yes C(8) C(9) C(10) 119.4(3) 1_555 1_555 1_555 yes C(8) C(9) C(14) 119.9(3) 1_555 1_555 1_555 yes C(10) C(9) C(14) 120.7(3) 1_555 1_555 1_555 yes C(9) C(10) C(11) 122.7(4) 1_555 1_555 1_555 yes C(10) C(11) C(12) 117.4(4) 1_555 1_555 1_555 yes N(2) C(12) C(11) 130.6(4) 1_555 1_555 1_555 yes N(2) C(12) C(13) 109.5(3) 1_555 1_555 1_555 yes C(11) C(12) C(13) 119.9(3) 1_555 1_555 1_555 yes N(1) C(13) C(12) 106.1(3) 1_555 1_555 1_555 yes N(1) C(13) C(14) 131.1(4) 1_555 1_555 1_555 yes C(12) C(13) C(14) 122.8(3) 1_555 1_555 1_555 yes C(1) C(14) C(9) 123.5(3) 1_555 1_555 1_555 yes C(1) C(14) C(13) 120.0(3) 1_555 1_555 1_555 yes C(9) C(14) C(13) 116.4(3) 1_555 1_555 1_555 yes N(1) C(15) N(2) 112.1(3) 1_555 1_555 1_555 yes N(1) C(15) C(16) 121.8(4) 1_555 1_555 1_555 yes N(2) C(15) C(16) 126.0(3) 1_555 1_555 1_555 yes C(15) C(16) C(17) 120.0(4) 1_555 1_555 1_555 yes C(15) C(16) C(21) 122.7(3) 1_555 1_555 1_555 yes C(17) C(16) C(21) 117.2(3) 1_555 1_555 1_555 yes C(16) C(17) C(18) 121.3(4) 1_555 1_555 1_555 yes C(17) C(18) C(19) 122.0(4) 1_555 1_555 1_555 yes N(3) C(19) C(18) 121.5(4) 1_555 1_555 1_555 yes N(3) C(19) C(20) 122.3(4) 1_555 1_555 1_555 yes C(18) C(19) C(20) 116.2(4) 1_555 1_555 1_555 yes C(19) C(20) C(21) 121.5(4) 1_555 1_555 1_555 yes C(16) C(21) C(20) 121.8(4) 1_555 1_555 1_555 yes N(3) C(22) C(23) 117.4(4) 1_555 1_555 1_555 yes N(3) C(24) C(25) 113.8(4) 1_555 1_555 1_555 yes #----------------------------------------------- #===============================================END data_6 _database_code_depnum_ccdc_archive 'CCDC 236775' _audit_creation_date 'Wed Oct 27 01:03:29 2004' _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 467.61 _chemical_formula_analytical ? _chemical_formula_sum ' C30 H33 N3 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 16.130(3) _cell_length_b 8.793(3) _cell_length_c 18.260(3) _cell_angle_alpha 90 _cell_angle_beta 96.12(1) _cell_angle_gamma 90 _cell_volume 2575.1(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.0 _cell_measurement_theta_max 14.4 _cell_measurement_temperature 296.2 #---------------------------------------------- _exptl_crystal_description prismatic _exptl_crystal_colour 'yellowish green' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000.00 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.920 _exptl_absorpt_correction_T_max 0.994 _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 4697 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 1.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.78 _reflns_number_total 4696 _reflns_number_gt 3272 _reflns_threshold_expression >2sigma(I) _diffrn_orient_matrix_UB_11 0.00760 _diffrn_orient_matrix_UB_12 -0.11061 _diffrn_orient_matrix_UB_13 0.01158 _diffrn_orient_matrix_UB_21 -0.05906 _diffrn_orient_matrix_UB_22 -0.01968 _diffrn_orient_matrix_UB_23 -0.02036 _diffrn_orient_matrix_UB_31 0.01852 _diffrn_orient_matrix_UB_32 -0.01765 _diffrn_orient_matrix_UB_33 -0.04985 #------------------------------------------- _refine_special_details ; Refinement F^2^ against All reflections. 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 refall _refine_ls_number_reflns 4696 _refine_ls_number_parameters 449 _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 0.0556 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.312 _refine_ls_shift/su_max 0.0004 _refine_diff_density_max 0.15 _refine_diff_density_min -0.14 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0082(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 0.0033 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H H 0.0000 0.0000 'International Tables Vol C Table 6.1.1.2' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O O 0.0106 0.0060 '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 0.14514(8) 0.1414(2) 0.84043(9) 0.0545(4) Uani 1.00 d . . . O(2) O 0.39087(10) 0.5331(2) 0.7970(1) 0.0906(6) Uani 1.00 d . . . N(1) N 0.04206(9) 0.3933(2) 0.86993(8) 0.0433(4) Uani 1.00 d . . . N(2) N 0.01003(9) 0.6327(2) 0.83434(9) 0.0472(5) Uani 1.00 d . . . N(3) N -0.3422(1) 0.4231(3) 0.9506(1) 0.0753(7) Uani 1.00 d . . . C(1) C 0.2113(1) 0.2422(2) 0.8682(1) 0.0427(5) Uani 1.00 d . . . C(2) C 0.2907(1) 0.1821(2) 0.8419(1) 0.0446(5) Uani 1.00 d . . . C(3) C 0.3079(1) 0.0275(2) 0.8465(1) 0.0533(6) Uani 1.00 d . . . C(4) C 0.3830(1) -0.0296(3) 0.8273(1) 0.0626(7) Uani 1.00 d . . . C(5) C 0.4421(1) 0.0674(3) 0.8040(1) 0.0648(7) Uani 1.00 d . . . C(6) C 0.4261(1) 0.2202(3) 0.7993(1) 0.0629(7) Uani 1.00 d . . . C(7) C 0.3506(1) 0.2794(2) 0.8176(1) 0.0506(6) Uani 1.00 d . . . C(8) C 0.3353(1) 0.4456(2) 0.8102(1) 0.0581(6) Uani 1.00 d . . . C(9) C 0.2501(1) 0.5004(2) 0.8168(1) 0.0479(6) Uani 1.00 d . . . C(10) C 0.2295(1) 0.6510(2) 0.7961(1) 0.0567(6) Uani 1.00 d . . . C(11) C 0.1515(1) 0.7101(2) 0.7994(1) 0.0561(6) Uani 1.00 d . . . C(12) C 0.0929(1) 0.6124(2) 0.8245(1) 0.0445(5) Uani 1.00 d . . . C(13) C 0.1117(1) 0.4632(2) 0.8465(1) 0.0410(5) Uani 1.00 d . . . C(14) C 0.1913(1) 0.4033(2) 0.84210(10) 0.0411(5) Uani 1.00 d . . . C(15) C -0.0173(1) 0.4978(2) 0.8624(1) 0.0439(5) Uani 1.00 d . . . C(16) C -0.1020(1) 0.4760(2) 0.8831(1) 0.0461(5) Uani 1.00 d . . . C(17) C -0.1725(1) 0.5219(3) 0.8383(1) 0.0522(6) Uani 1.00 d . . . C(18) C -0.2513(1) 0.5020(3) 0.8599(1) 0.0580(7) Uani 1.00 d . . . C(19) C -0.2633(1) 0.4346(3) 0.9274(1) 0.0556(6) Uani 1.00 d . . . C(20) C -0.1918(1) 0.3851(3) 0.9712(1) 0.0556(6) Uani 1.00 d . . . C(21) C -0.1135(1) 0.4055(2) 0.9494(1) 0.0508(6) Uani 1.00 d . . . C(22) C -0.4144(1) 0.4871(4) 0.9053(2) 0.086(1) Uani 1.00 d . . . C(23) C -0.4218(2) 0.6561(5) 0.9128(3) 0.108(1) Uani 1.00 d . . . C(24) C -0.3601(2) 0.3072(5) 1.0036(2) 0.092(1) Uani 1.00 d . . . C(25) C -0.3783(3) 0.1555(6) 0.9704(3) 0.130(2) Uani 1.00 d . . . C(26) C 0.2207(2) 0.2400(3) 0.9526(1) 0.0616(7) Uani 1.00 d . . . C(27) C -0.0321(1) 0.7814(2) 0.8282(1) 0.0526(6) Uani 1.00 d . . . C(28) C -0.0196(2) 0.8706(3) 0.8982(1) 0.0732(8) Uani 1.00 d . . . C(29) C -0.0649(2) 1.0226(3) 0.8910(2) 0.091(1) Uani 1.00 d . . . C(30) C -0.1589(3) 1.0047(5) 0.8817(2) 0.107(1) Uani 1.00 d . . . H(1) H 0.098(1) 0.188(3) 0.852(1) 0.085(8) Uiso 1.00 calc . . . H(2) H 0.267(1) -0.044(2) 0.864(1) 0.054(6) Uiso 1.00 calc . . . H(3) H 0.393(1) -0.143(3) 0.830(1) 0.071(7) Uiso 1.00 calc . . . H(4) H 0.495(1) 0.028(3) 0.791(1) 0.068(6) Uiso 1.00 calc . . . H(5) H 0.464(1) 0.291(3) 0.782(1) 0.082(8) Uiso 1.00 calc . . . H(6) H 0.273(1) 0.710(3) 0.778(1) 0.073(7) Uiso 1.00 calc . . . H(7) H 0.139(1) 0.812(3) 0.784(1) 0.060(6) Uiso 1.00 calc . . . H(8) H -0.168(1) 0.565(2) 0.792(1) 0.051(6) Uiso 1.00 calc . . . H(9) H -0.296(1) 0.532(2) 0.826(1) 0.064(6) Uiso 1.00 calc . . . H(10) H -0.197(1) 0.333(3) 1.019(1) 0.070(7) Uiso 1.00 calc . . . H(11) H -0.063(1) 0.372(2) 0.982(1) 0.049(5) Uiso 1.00 calc . . . H(12) H -0.412(2) 0.451(3) 0.850(2) 0.098(9) Uiso 1.00 calc . . . H(13) H -0.463(2) 0.435(3) 0.920(1) 0.099(9) Uiso 1.00 calc . . . H(14) H -0.475(2) 0.688(4) 0.884(2) 0.14(1) Uiso 1.00 calc . . . H(15) H -0.428(2) 0.683(4) 0.969(2) 0.12(1) Uiso 1.00 calc . . . H(16) H -0.371(2) 0.715(3) 0.899(2) 0.108(9) Uiso 1.00 calc . . . H(17) H -0.312(2) 0.305(3) 1.043(2) 0.108(9) Uiso 1.00 calc . . . H(18) H -0.409(2) 0.340(3) 1.028(1) 0.096(8) Uiso 1.00 calc . . . H(19) H -0.437(2) 0.165(4) 0.932(2) 0.17(1) Uiso 1.00 calc . . . H(20) H -0.397(2) 0.079(5) 1.003(2) 0.17(1) Uiso 1.00 calc . . . H(21) H -0.342(3) 0.125(5) 0.937(3) 0.19(2) Uiso 1.00 calc . . . H(22) H 0.267(2) 0.310(3) 0.974(2) 0.100(9) Uiso 1.00 calc . . . H(23) H 0.170(1) 0.280(3) 0.970(1) 0.068(6) Uiso 1.00 calc . . . H(24) H 0.230(1) 0.129(3) 0.970(1) 0.089(8) Uiso 1.00 calc . . . H(25) H -0.007(1) 0.834(3) 0.788(1) 0.076(7) Uiso 1.00 calc . . . H(26) H -0.089(1) 0.764(3) 0.808(1) 0.072(7) Uiso 1.00 calc . . . H(27) H -0.043(1) 0.801(3) 0.936(1) 0.089(8) Uiso 1.00 calc . . . H(28) H 0.038(2) 0.881(3) 0.916(2) 0.100(9) Uiso 1.00 calc . . . H(29) H -0.052(2) 1.084(4) 0.843(2) 0.15(1) Uiso 1.00 calc . . . H(30) H -0.043(2) 1.085(4) 0.936(2) 0.16(1) Uiso 1.00 calc . . . H(31) H -0.189(2) 1.099(4) 0.877(2) 0.14(1) Uiso 1.00 calc . . . H(32) H -0.148(2) 0.981(5) 0.937(2) 0.17(1) Uiso 1.00 calc . . . H(33) H -0.198(2) 0.925(4) 0.879(2) 0.13(1) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(1) 0.0370(7) 0.0419(7) 0.086(1) -0.0022(6) 0.0138(7) -0.0065(7) O(2) 0.0558(10) 0.065(1) 0.157(2) -0.0148(8) 0.040(1) 0.009(1) N(1) 0.0379(8) 0.0410(8) 0.0517(9) 0.0049(7) 0.0082(7) -0.0013(7) N(2) 0.0452(9) 0.0398(9) 0.0559(10) 0.0076(7) 0.0028(7) -0.0011(8) N(3) 0.0403(10) 0.107(2) 0.080(1) 0.005(1) 0.0145(9) 0.005(1) C(1) 0.0361(9) 0.0406(10) 0.052(1) -0.0016(8) 0.0070(8) -0.0029(9) C(2) 0.0371(9) 0.047(1) 0.050(1) 0.0015(8) 0.0035(8) -0.0054(9) C(3) 0.042(1) 0.051(1) 0.067(1) 0.0043(9) 0.0070(10) -0.002(1) C(4) 0.047(1) 0.056(1) 0.085(2) 0.011(1) 0.006(1) -0.011(1) C(5) 0.039(1) 0.071(2) 0.085(2) 0.009(1) 0.012(1) -0.017(1) C(6) 0.040(1) 0.071(2) 0.079(2) -0.004(1) 0.016(1) -0.011(1) C(7) 0.0356(10) 0.054(1) 0.063(1) -0.0027(9) 0.0085(9) -0.008(1) C(8) 0.045(1) 0.057(1) 0.075(1) -0.0076(10) 0.014(1) -0.001(1) C(9) 0.044(1) 0.044(1) 0.058(1) -0.0069(8) 0.0110(9) -0.0038(9) C(10) 0.053(1) 0.046(1) 0.073(1) -0.0099(10) 0.014(1) 0.003(1) C(11) 0.059(1) 0.040(1) 0.069(1) -0.0012(10) 0.007(1) 0.005(1) C(12) 0.045(1) 0.041(1) 0.047(1) 0.0033(8) 0.0014(8) -0.0012(8) C(13) 0.0377(9) 0.0398(10) 0.046(1) 0.0000(8) 0.0059(8) -0.0014(8) C(14) 0.0399(10) 0.0384(10) 0.0450(10) -0.0012(8) 0.0052(8) -0.0044(8) C(15) 0.0425(10) 0.043(1) 0.046(1) 0.0032(8) 0.0040(8) -0.0030(9) C(16) 0.0410(10) 0.045(1) 0.053(1) 0.0065(8) 0.0061(8) -0.0076(9) C(17) 0.045(1) 0.064(1) 0.048(1) 0.0084(10) 0.0053(9) -0.003(1) C(18) 0.040(1) 0.078(2) 0.055(1) 0.012(1) 0.0014(9) -0.006(1) C(19) 0.044(1) 0.065(1) 0.059(1) 0.0044(10) 0.0101(9) -0.009(1) C(20) 0.047(1) 0.064(1) 0.057(1) 0.0057(10) 0.0115(10) 0.001(1) C(21) 0.042(1) 0.052(1) 0.058(1) 0.0100(9) 0.0025(9) -0.0013(10) C(22) 0.039(1) 0.124(3) 0.095(2) 0.003(1) 0.008(1) 0.001(2) C(23) 0.062(2) 0.135(3) 0.128(3) 0.033(2) 0.015(2) 0.003(3) C(24) 0.054(2) 0.154(3) 0.068(2) -0.011(2) 0.017(1) 0.008(2) C(25) 0.129(4) 0.122(4) 0.134(4) -0.024(3) -0.001(3) 0.031(3) C(26) 0.069(2) 0.064(1) 0.053(1) 0.021(1) 0.015(1) 0.007(1) C(27) 0.056(1) 0.043(1) 0.057(1) 0.0117(10) -0.001(1) 0.000(1) C(28) 0.093(2) 0.056(1) 0.066(2) 0.021(1) -0.012(1) -0.012(1) C(29) 0.120(3) 0.061(2) 0.090(2) 0.032(2) -0.007(2) -0.019(2) C(30) 0.117(3) 0.094(3) 0.118(3) 0.048(2) 0.046(2) 0.022(2) #--------------------------------------------------- _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) 1.438(2) 1_555 1_555 yes O(2) C(8) 1.224(2) 1_555 1_555 yes N(1) C(13) 1.388(2) 1_555 1_555 yes N(1) C(15) 1.324(2) 1_555 1_555 yes N(2) C(12) 1.380(2) 1_555 1_555 yes N(2) C(15) 1.383(2) 1_555 1_555 yes N(2) C(27) 1.472(2) 1_555 1_555 yes N(3) C(19) 1.387(3) 1_555 1_555 yes N(3) C(22) 1.467(3) 1_555 1_555 yes N(3) C(24) 1.456(4) 1_555 1_555 yes C(1) C(2) 1.510(2) 1_555 1_555 yes C(1) C(14) 1.518(3) 1_555 1_555 yes C(1) C(26) 1.532(3) 1_555 1_555 yes C(2) C(3) 1.388(3) 1_555 1_555 yes C(2) C(7) 1.398(3) 1_555 1_555 yes C(3) C(4) 1.389(3) 1_555 1_555 yes C(4) C(5) 1.380(3) 1_555 1_555 yes C(5) C(6) 1.369(3) 1_555 1_555 yes C(6) C(7) 1.398(3) 1_555 1_555 yes C(7) C(8) 1.485(3) 1_555 1_555 yes C(8) C(9) 1.475(3) 1_555 1_555 yes C(9) C(10) 1.408(3) 1_555 1_555 yes C(9) C(14) 1.390(2) 1_555 1_555 yes C(10) C(11) 1.370(3) 1_555 1_555 yes C(11) C(12) 1.389(3) 1_555 1_555 yes C(12) C(13) 1.396(3) 1_555 1_555 yes C(13) C(14) 1.398(2) 1_555 1_555 yes C(15) C(16) 1.469(2) 1_555 1_555 yes C(16) C(17) 1.388(3) 1_555 1_555 yes C(16) C(21) 1.389(3) 1_555 1_555 yes C(17) C(18) 1.382(3) 1_555 1_555 yes C(18) C(19) 1.400(3) 1_555 1_555 yes C(19) C(20) 1.401(3) 1_555 1_555 yes C(20) C(21) 1.376(3) 1_555 1_555 yes C(22) C(23) 1.499(5) 1_555 1_555 yes C(24) C(25) 1.482(6) 1_555 1_555 yes C(27) C(28) 1.495(3) 1_555 1_555 yes C(28) C(29) 1.523(3) 1_555 1_555 yes C(29) C(30) 1.516(6) 1_555 1_555 yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(13) N(1) C(15) 105.1(2) 1_555 1_555 1_555 yes C(12) N(2) C(15) 106.8(1) 1_555 1_555 1_555 yes C(12) N(2) C(27) 123.4(2) 1_555 1_555 1_555 yes C(15) N(2) C(27) 128.9(2) 1_555 1_555 1_555 yes C(19) N(3) C(22) 119.9(2) 1_555 1_555 1_555 yes C(19) N(3) C(24) 120.5(2) 1_555 1_555 1_555 yes C(22) N(3) C(24) 116.3(2) 1_555 1_555 1_555 yes O(1) C(1) C(2) 107.1(1) 1_555 1_555 1_555 yes O(1) C(1) C(14) 109.8(1) 1_555 1_555 1_555 yes O(1) C(1) C(26) 109.7(2) 1_555 1_555 1_555 yes C(2) C(1) C(14) 112.7(1) 1_555 1_555 1_555 yes C(2) C(1) C(26) 108.6(2) 1_555 1_555 1_555 yes C(14) C(1) C(26) 108.8(2) 1_555 1_555 1_555 yes C(1) C(2) C(3) 119.7(2) 1_555 1_555 1_555 yes C(1) C(2) C(7) 121.6(2) 1_555 1_555 1_555 yes C(3) C(2) C(7) 118.6(2) 1_555 1_555 1_555 yes C(2) C(3) C(4) 120.8(2) 1_555 1_555 1_555 yes C(3) C(4) C(5) 120.3(2) 1_555 1_555 1_555 yes C(4) C(5) C(6) 119.6(2) 1_555 1_555 1_555 yes C(5) C(6) C(7) 120.9(2) 1_555 1_555 1_555 yes C(2) C(7) C(6) 119.8(2) 1_555 1_555 1_555 yes C(2) C(7) C(8) 121.2(2) 1_555 1_555 1_555 yes C(6) C(7) C(8) 119.0(2) 1_555 1_555 1_555 yes O(2) C(8) C(7) 121.3(2) 1_555 1_555 1_555 yes O(2) C(8) C(9) 121.3(2) 1_555 1_555 1_555 yes C(7) C(8) C(9) 117.4(2) 1_555 1_555 1_555 yes C(8) C(9) C(10) 118.7(2) 1_555 1_555 1_555 yes C(8) C(9) C(14) 120.1(2) 1_555 1_555 1_555 yes C(10) C(9) C(14) 121.2(2) 1_555 1_555 1_555 yes C(9) C(10) C(11) 122.4(2) 1_555 1_555 1_555 yes C(10) C(11) C(12) 116.2(2) 1_555 1_555 1_555 yes N(2) C(12) C(11) 131.7(2) 1_555 1_555 1_555 yes N(2) C(12) C(13) 105.5(2) 1_555 1_555 1_555 yes C(11) C(12) C(13) 122.8(2) 1_555 1_555 1_555 yes N(1) C(13) C(12) 110.3(2) 1_555 1_555 1_555 yes N(1) C(13) C(14) 129.0(2) 1_555 1_555 1_555 yes C(12) C(13) C(14) 120.7(2) 1_555 1_555 1_555 yes C(1) C(14) C(9) 123.2(2) 1_555 1_555 1_555 yes C(1) C(14) C(13) 120.0(2) 1_555 1_555 1_555 yes C(9) C(14) C(13) 116.8(2) 1_555 1_555 1_555 yes N(1) C(15) N(2) 112.2(2) 1_555 1_555 1_555 yes N(1) C(15) C(16) 124.4(2) 1_555 1_555 1_555 yes N(2) C(15) C(16) 123.3(2) 1_555 1_555 1_555 yes C(15) C(16) C(17) 122.4(2) 1_555 1_555 1_555 yes C(15) C(16) C(21) 119.8(2) 1_555 1_555 1_555 yes C(17) C(16) C(21) 117.8(2) 1_555 1_555 1_555 yes C(16) C(17) C(18) 121.1(2) 1_555 1_555 1_555 yes C(17) C(18) C(19) 121.5(2) 1_555 1_555 1_555 yes N(3) C(19) C(18) 121.2(2) 1_555 1_555 1_555 yes N(3) C(19) C(20) 121.9(2) 1_555 1_555 1_555 yes C(18) C(19) C(20) 116.9(2) 1_555 1_555 1_555 yes C(19) C(20) C(21) 121.3(2) 1_555 1_555 1_555 yes C(16) C(21) C(20) 121.4(2) 1_555 1_555 1_555 yes N(3) C(22) C(23) 113.3(3) 1_555 1_555 1_555 yes N(3) C(24) C(25) 113.8(3) 1_555 1_555 1_555 yes N(2) C(27) C(28) 112.4(2) 1_555 1_555 1_555 yes C(27) C(28) C(29) 111.5(2) 1_555 1_555 1_555 yes C(28) C(29) C(30) 112.5(3) 1_555 1_555 1_555 yes #--------------------------------------------------- #===============================================END data_7 _database_code_depnum_ccdc_archive 'CCDC 236776' _audit_creation_date 'Fri Oct 29 16:04:33 2004' _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 467.61 _chemical_formula_analytical ? _chemical_formula_sum ' C30 H33 N3 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 12.007(3) _cell_length_b 13.152(4) _cell_length_c 16.196(5) _cell_angle_alpha 90 _cell_angle_beta 102.99(2) _cell_angle_gamma 90 _cell_volume 2492(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3 _cell_measurement_theta_min 11.5 _cell_measurement_theta_max 12.2 _cell_measurement_temperature 296.2 #----------------------------------------------------------- _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000.00 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.929 _exptl_absorpt_correction_T_max 0.998 _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 4766 _diffrn_reflns_av_R_equivalents 0.095 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.23 _reflns_number_total 4390 _reflns_number_gt 1453 _reflns_threshold_expression >2sigma(I) _diffrn_orient_matrix_UB_11 0.06679 _diffrn_orient_matrix_UB_12 0.04260 _diffrn_orient_matrix_UB_13 -0.00587 _diffrn_orient_matrix_UB_21 0.04882 _diffrn_orient_matrix_UB_22 -0.06231 _diffrn_orient_matrix_UB_23 0.00528 _diffrn_orient_matrix_UB_31 -0.02150 _diffrn_orient_matrix_UB_32 -0.00918 _diffrn_orient_matrix_UB_33 -0.06287 #------------------------------------------------------------------------------ _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 refall _refine_ls_number_reflns 4390 _refine_ls_number_parameters 449 _refine_ls_goodness_of_fit_ref 1.068 _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 0.2316 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2316 _refine_ls_wR_factor_gt 0.1490 _refine_ls_shift/su_max 0.0003 _refine_diff_density_max 0.43 _refine_diff_density_min -0.42 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0036(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 0.0033 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H H 0.0000 0.0000 'International Tables Vol C Table 6.1.1.2' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O O 0.0106 0.0060 '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 1.2026(4) 0.6215(3) 0.9263(3) 0.042(1) Uani 1.00 d . . . O(2) O 1.0823(5) 0.3839(4) 1.1628(3) 0.066(2) Uani 1.00 d . . . N(1) N 0.9761(4) 0.2472(4) 1.0304(3) 0.035(2) Uani 1.00 d . . . N(2) N 0.9674(4) 0.1897(4) 0.8981(3) 0.035(2) Uani 1.00 d . . . N(3) N 0.6257(5) -0.1230(4) 1.0442(3) 0.048(2) Uani 1.00 d . . . C(1) C 1.1194(5) 0.4327(5) 1.1095(4) 0.035(2) Uani 1.00 d . . . C(2) C 1.1822(6) 0.5296(5) 1.1352(4) 0.037(2) Uani 1.00 d . . . C(3) C 1.1917(7) 0.5672(6) 1.2176(5) 0.046(2) Uani 1.00 d . . . C(4) C 1.2498(7) 0.6572(6) 1.2422(5) 0.050(3) Uani 1.00 d . . . C(5) C 1.2961(6) 0.7120(6) 1.1842(5) 0.046(2) Uani 1.00 d . . . C(6) C 1.2867(6) 0.6747(6) 1.1045(5) 0.040(2) Uani 1.00 d . . . C(7) C 1.2306(6) 0.5845(5) 1.0780(4) 0.036(2) Uani 1.00 d . . . C(8) C 1.2316(6) 0.5442(5) 0.9896(4) 0.037(2) Uani 1.00 d . . . C(9) C 1.1563(5) 0.4500(5) 0.9641(4) 0.035(2) Uani 1.00 d . . . C(10) C 1.1445(6) 0.4151(5) 0.8818(4) 0.040(2) Uani 1.00 d . . . C(11) C 1.0873(6) 0.3285(6) 0.8526(4) 0.038(2) Uani 1.00 d . . . C(12) C 1.0359(5) 0.2762(5) 0.9081(4) 0.034(2) Uani 1.00 d . . . C(13) C 1.0421(5) 0.3096(5) 0.9914(4) 0.032(2) Uani 1.00 d . . . C(14) C 1.1052(5) 0.3978(5) 1.0213(4) 0.032(2) Uani 1.00 d . . . C(15) C 0.9324(5) 0.1756(5) 0.9737(4) 0.034(2) Uani 1.00 d . . . C(16) C 0.8543(6) 0.0973(5) 0.9883(4) 0.036(2) Uani 1.00 d . . . C(17) C 0.8476(6) -0.0008(5) 0.9544(5) 0.040(2) Uani 1.00 d . . . C(18) C 0.7744(6) -0.0736(6) 0.9724(5) 0.043(2) Uani 1.00 d . . . C(19) C 0.7004(6) -0.0512(5) 1.0258(4) 0.039(2) Uani 1.00 d . . . C(20) C 0.7071(6) 0.0471(5) 1.0613(4) 0.036(2) Uani 1.00 d . . . C(21) C 0.7817(6) 0.1180(5) 1.0425(4) 0.038(2) Uani 1.00 d . . . C(22) C 0.6215(8) -0.2251(6) 1.0095(6) 0.053(2) Uani 1.00 d . . . C(23) C 0.546(1) -0.2308(8) 0.9210(7) 0.080(3) Uani 1.00 d . . . C(24) C 0.5517(7) -0.1028(7) 1.1037(6) 0.060(3) Uani 1.00 d . . . C(25) C 0.613(1) -0.1159(9) 1.1942(7) 0.084(4) Uani 1.00 d . . . C(26) C 1.3574(6) 0.5164(6) 0.9905(5) 0.043(2) Uani 1.00 d . . . C(27) C 0.9384(6) 0.1327(6) 0.8183(5) 0.039(2) Uani 1.00 d . . . C(28) C 1.0311(6) 0.0570(6) 0.8114(5) 0.042(2) Uani 1.00 d . . . C(29) C 1.0067(7) 0.0027(6) 0.7263(5) 0.050(2) Uani 1.00 d . . . C(30) C 1.0804(8) -0.0912(7) 0.7272(6) 0.062(3) Uani 1.00 d . . . H(1) H 1.13(1) 0.67(1) 0.938(9) 0.272(2) Uiso 1.00 calc . . . H(2) H 1.159(5) 0.528(4) 1.252(4) 0.039(8) Uiso 1.00 calc . . . H(3) H 1.264(5) 0.679(5) 1.294(4) 0.039(8) Uiso 1.00 calc . . . H(4) H 1.344(5) 0.774(5) 1.206(4) 0.067(7) Uiso 1.00 calc . . . H(5) H 1.323(5) 0.717(5) 1.066(4) 0.048(8) Uiso 1.00 calc . . . H(6) H 1.176(5) 0.457(4) 0.839(4) 0.044(8) Uiso 1.00 calc . . . H(7) H 1.082(5) 0.303(4) 0.790(4) 0.046(8) Uiso 1.00 calc . . . H(8) H 0.900(4) -0.022(4) 0.917(3) 0.035(9) Uiso 1.00 calc . . . H(9) H 0.779(5) -0.145(5) 0.949(3) 0.040(8) Uiso 1.00 calc . . . H(10) H 0.667(5) 0.062(5) 1.101(4) 0.056(7) Uiso 1.00 calc . . . H(11) H 0.780(4) 0.186(4) 1.071(3) 0.024(9) Uiso 1.00 calc . . . H(12) H 0.596(6) -0.277(6) 1.043(4) 0.077(6) Uiso 1.00 calc . . . H(13) H 0.709(6) -0.248(6) 1.011(4) 0.080(6) Uiso 1.00 calc . . . H(14) H 0.459(8) -0.218(8) 0.924(6) 0.137(4) Uiso 1.00 calc . . . H(15) H 0.564(10) -0.183(8) 0.887(7) 0.149(3) Uiso 1.00 calc . . . H(16) H 0.557(7) -0.286(6) 0.890(5) 0.082(6) Uiso 1.00 calc . . . H(17) H 0.483(5) -0.159(5) 1.093(4) 0.061(7) Uiso 1.00 calc . . . H(18) H 0.512(7) -0.024(6) 1.098(5) 0.105(5) Uiso 1.00 calc . . . H(19) H 0.687(6) -0.054(6) 1.206(4) 0.076(7) Uiso 1.00 calc . . . H(20) H 0.559(9) -0.103(8) 1.222(6) 0.136(4) Uiso 1.00 calc . . . H(21) H 0.645(6) -0.193(6) 1.211(5) 0.091(5) Uiso 1.00 calc . . . H(22) H 1.401(7) 0.591(7) 1.001(5) 0.135(4) Uiso 1.00 calc . . . H(23) H 1.358(5) 0.481(4) 0.934(4) 0.033(9) Uiso 1.00 calc . . . H(24) H 1.393(6) 0.453(6) 1.032(5) 0.095(6) Uiso 1.00 calc . . . H(25) H 0.933(5) 0.185(5) 0.767(4) 0.054(8) Uiso 1.00 calc . . . H(26) H 0.860(5) 0.099(4) 0.814(3) 0.032(9) Uiso 1.00 calc . . . H(27) H 1.040(5) 0.002(5) 0.856(4) 0.052(8) Uiso 1.00 calc . . . H(28) H 1.108(6) 0.092(5) 0.824(4) 0.057(7) Uiso 1.00 calc . . . H(29) H 0.930(6) -0.027(6) 0.716(5) 0.083(6) Uiso 1.00 calc . . . H(30) H 1.025(5) 0.055(5) 0.687(4) 0.054(7) Uiso 1.00 calc . . . H(31) H 1.165(8) -0.075(7) 0.741(6) 0.130(4) Uiso 1.00 calc . . . H(32) H 1.092(6) -0.123(6) 0.677(5) 0.086(6) Uiso 1.00 calc . . . H(33) H 1.074(6) -0.145(5) 0.778(4) 0.079(6) 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) 0.054(3) 0.032(3) 0.040(3) -0.001(2) 0.014(2) 0.004(2) O(2) 0.101(4) 0.065(4) 0.039(3) -0.034(3) 0.030(3) 0.005(3) N(1) 0.035(3) 0.035(3) 0.040(3) -0.001(3) 0.017(3) 0.002(2) N(2) 0.033(3) 0.036(3) 0.039(3) -0.001(2) 0.012(3) -0.002(2) N(3) 0.064(4) 0.034(3) 0.051(4) -0.018(3) 0.026(3) -0.007(3) C(1) 0.026(4) 0.043(4) 0.035(3) -0.001(3) 0.003(3) -0.006(3) C(2) 0.037(4) 0.035(4) 0.038(3) 0.001(3) 0.007(3) 0.000(3) C(3) 0.058(5) 0.041(4) 0.039(4) 0.002(4) 0.013(4) 0.000(3) C(4) 0.072(6) 0.043(5) 0.035(4) -0.001(4) 0.010(4) -0.009(3) C(5) 0.049(5) 0.042(5) 0.046(4) 0.006(4) 0.006(4) -0.002(3) C(6) 0.040(4) 0.034(4) 0.045(4) 0.000(3) 0.006(4) 0.004(3) C(7) 0.034(4) 0.032(4) 0.042(4) 0.007(3) 0.008(3) 0.001(3) C(8) 0.040(3) 0.029(4) 0.044(4) -0.003(3) 0.014(4) 0.004(2) C(9) 0.034(4) 0.034(4) 0.039(3) -0.002(3) 0.013(3) 0.002(3) C(10) 0.045(5) 0.042(4) 0.038(4) -0.006(3) 0.017(4) 0.005(3) C(11) 0.043(4) 0.049(4) 0.023(4) -0.006(3) 0.008(3) -0.006(3) C(12) 0.035(4) 0.033(4) 0.038(3) 0.004(3) 0.016(3) -0.002(3) C(13) 0.033(4) 0.031(4) 0.036(3) 0.003(3) 0.014(3) -0.001(3) C(14) 0.033(4) 0.029(4) 0.035(3) 0.004(3) 0.007(3) 0.003(2) C(15) 0.027(4) 0.036(4) 0.041(3) 0.006(3) 0.010(3) 0.002(3) C(16) 0.034(4) 0.037(3) 0.035(4) -0.004(3) 0.004(3) 0.002(3) C(17) 0.042(4) 0.040(3) 0.040(4) -0.001(3) 0.018(4) -0.005(3) C(18) 0.050(5) 0.037(4) 0.049(5) -0.004(3) 0.024(3) -0.005(4) C(19) 0.045(4) 0.035(3) 0.038(4) 0.000(3) 0.010(3) 0.001(3) C(20) 0.038(4) 0.040(4) 0.034(4) -0.005(3) 0.016(3) -0.006(3) C(21) 0.041(4) 0.031(4) 0.046(4) 0.000(3) 0.017(3) -0.004(4) C(22) 0.068(6) 0.028(3) 0.066(5) -0.011(4) 0.023(4) 0.001(4) C(23) 0.102(8) 0.061(7) 0.070(6) -0.001(7) 0.004(5) -0.036(6) C(24) 0.054(6) 0.064(6) 0.070(4) -0.020(5) 0.034(4) -0.014(5) C(25) 0.114(10) 0.074(7) 0.068(5) -0.044(7) 0.025(6) 0.001(6) C(26) 0.038(4) 0.045(5) 0.047(5) 0.000(4) 0.008(4) -0.016(4) C(27) 0.034(4) 0.044(4) 0.039(4) -0.004(3) 0.006(4) -0.010(3) C(28) 0.037(4) 0.049(5) 0.038(4) 0.004(3) 0.004(4) -0.004(3) C(29) 0.061(6) 0.044(5) 0.044(4) -0.003(4) 0.008(5) -0.011(3) C(30) 0.079(6) 0.050(6) 0.063(6) 0.013(4) 0.028(6) -0.018(4) #--------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(8) 1.429(8) 1_555 1_555 yes O(2) C(1) 1.237(8) 1_555 1_555 yes N(1) C(13) 1.388(7) 1_555 1_555 yes N(1) C(15) 1.337(8) 1_555 1_555 yes N(2) C(12) 1.392(8) 1_555 1_555 yes N(2) C(15) 1.392(8) 1_555 1_555 yes N(2) C(27) 1.467(8) 1_555 1_555 yes N(3) C(19) 1.380(8) 1_555 1_555 yes N(3) C(22) 1.453(9) 1_555 1_555 yes N(3) C(24) 1.474(9) 1_555 1_555 yes C(1) C(2) 1.492(9) 1_555 1_555 yes C(1) C(14) 1.473(9) 1_555 1_555 yes C(2) C(3) 1.405(9) 1_555 1_555 yes C(2) C(7) 1.398(9) 1_555 1_555 yes C(3) C(4) 1.39(1) 1_555 1_555 yes C(4) C(5) 1.40(1) 1_555 1_555 yes C(5) C(6) 1.362(10) 1_555 1_555 yes C(6) C(7) 1.383(9) 1_555 1_555 yes C(7) C(8) 1.530(9) 1_555 1_555 yes C(8) C(9) 1.535(9) 1_555 1_555 yes C(8) C(26) 1.551(10) 1_555 1_555 yes C(9) C(10) 1.388(9) 1_555 1_555 yes C(9) C(14) 1.400(8) 1_555 1_555 yes C(10) C(11) 1.358(9) 1_555 1_555 yes C(11) C(12) 1.383(9) 1_555 1_555 yes C(12) C(13) 1.406(8) 1_555 1_555 yes C(13) C(14) 1.410(9) 1_555 1_555 yes C(15) C(16) 1.448(9) 1_555 1_555 yes C(16) C(17) 1.397(9) 1_555 1_555 yes C(16) C(21) 1.397(9) 1_555 1_555 yes C(17) C(18) 1.375(9) 1_555 1_555 yes C(18) C(19) 1.403(9) 1_555 1_555 yes C(19) C(20) 1.409(9) 1_555 1_555 yes C(20) C(21) 1.373(9) 1_555 1_555 yes C(22) C(23) 1.52(1) 1_555 1_555 yes C(24) C(25) 1.50(1) 1_555 1_555 yes C(27) C(28) 1.516(10) 1_555 1_555 yes C(28) C(29) 1.521(10) 1_555 1_555 yes C(29) C(30) 1.52(1) 1_555 1_555 yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(13) N(1) C(15) 106.2(5) 1_555 1_555 1_555 yes C(12) N(2) C(15) 107.0(5) 1_555 1_555 1_555 yes C(12) N(2) C(27) 122.4(6) 1_555 1_555 1_555 yes C(15) N(2) C(27) 130.4(6) 1_555 1_555 1_555 yes C(19) N(3) C(22) 121.1(6) 1_555 1_555 1_555 yes C(19) N(3) C(24) 122.2(6) 1_555 1_555 1_555 yes C(22) N(3) C(24) 116.5(6) 1_555 1_555 1_555 yes O(2) C(1) C(2) 119.2(6) 1_555 1_555 1_555 yes O(2) C(1) C(14) 122.2(7) 1_555 1_555 1_555 yes C(2) C(1) C(14) 118.6(6) 1_555 1_555 1_555 yes C(1) C(2) C(3) 119.6(6) 1_555 1_555 1_555 yes C(1) C(2) C(7) 121.0(7) 1_555 1_555 1_555 yes C(3) C(2) C(7) 119.4(7) 1_555 1_555 1_555 yes C(2) C(3) C(4) 120.2(7) 1_555 1_555 1_555 yes C(3) C(4) C(5) 119.9(8) 1_555 1_555 1_555 yes C(4) C(5) C(6) 119.5(7) 1_555 1_555 1_555 yes C(5) C(6) C(7) 122.2(7) 1_555 1_555 1_555 yes C(2) C(7) C(6) 118.9(7) 1_555 1_555 1_555 yes C(2) C(7) C(8) 122.2(6) 1_555 1_555 1_555 yes C(6) C(7) C(8) 118.8(6) 1_555 1_555 1_555 yes O(1) C(8) C(7) 111.9(5) 1_555 1_555 1_555 yes O(1) C(8) C(9) 110.3(6) 1_555 1_555 1_555 yes O(1) C(8) C(26) 104.8(6) 1_555 1_555 1_555 yes C(7) C(8) C(9) 113.8(6) 1_555 1_555 1_555 yes C(7) C(8) C(26) 106.6(6) 1_555 1_555 1_555 yes C(9) C(8) C(26) 109.0(6) 1_555 1_555 1_555 yes C(8) C(9) C(10) 116.9(6) 1_555 1_555 1_555 yes C(8) C(9) C(14) 122.5(6) 1_555 1_555 1_555 yes C(10) C(9) C(14) 120.6(7) 1_555 1_555 1_555 yes C(9) C(10) C(11) 123.1(7) 1_555 1_555 1_555 yes C(10) C(11) C(12) 117.1(7) 1_555 1_555 1_555 yes N(2) C(12) C(11) 132.0(6) 1_555 1_555 1_555 yes N(2) C(12) C(13) 105.6(6) 1_555 1_555 1_555 yes C(11) C(12) C(13) 122.3(7) 1_555 1_555 1_555 yes N(1) C(13) C(12) 109.8(6) 1_555 1_555 1_555 yes N(1) C(13) C(14) 130.4(6) 1_555 1_555 1_555 yes C(12) C(13) C(14) 119.7(6) 1_555 1_555 1_555 yes C(1) C(14) C(9) 121.1(6) 1_555 1_555 1_555 yes C(1) C(14) C(13) 121.7(6) 1_555 1_555 1_555 yes C(9) C(14) C(13) 117.2(6) 1_555 1_555 1_555 yes N(1) C(15) N(2) 111.2(6) 1_555 1_555 1_555 yes N(1) C(15) C(16) 123.9(6) 1_555 1_555 1_555 yes N(2) C(15) C(16) 124.9(6) 1_555 1_555 1_555 yes C(15) C(16) C(17) 125.1(7) 1_555 1_555 1_555 yes C(15) C(16) C(21) 118.8(6) 1_555 1_555 1_555 yes C(17) C(16) C(21) 116.0(7) 1_555 1_555 1_555 yes C(16) C(17) C(18) 122.9(7) 1_555 1_555 1_555 yes C(17) C(18) C(19) 120.5(7) 1_555 1_555 1_555 yes N(3) C(19) C(18) 121.3(7) 1_555 1_555 1_555 yes N(3) C(19) C(20) 121.4(6) 1_555 1_555 1_555 yes C(18) C(19) C(20) 117.3(7) 1_555 1_555 1_555 yes C(19) C(20) C(21) 120.9(6) 1_555 1_555 1_555 yes C(16) C(21) C(20) 122.5(7) 1_555 1_555 1_555 yes N(3) C(22) C(23) 111.9(7) 1_555 1_555 1_555 yes N(3) C(24) C(25) 112.4(8) 1_555 1_555 1_555 yes N(2) C(27) C(28) 111.6(6) 1_555 1_555 1_555 yes C(27) C(28) C(29) 112.3(7) 1_555 1_555 1_555 yes C(28) C(29) C(30) 112.4(7) 1_555 1_555 1_555 yes #--------------------------------------------------- #===============================================END