# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 207/335 data_master_file_afc7*.xtl #------------------------------------------------------------------------------ _audit_creation_date 'Thu Jan 21 13:36:02 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 437.49 _chemical_formula_analytical ? _chemical_formula_sum 'C25 H27 N O6 ' _chemical_formula_moiety 'C25 H27 N O6 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 12.749(2) _cell_length_b 16.163(2) _cell_length_c 10.624(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2189.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 29.1 _cell_measurement_theta_max 30.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_Int_Tables_number 33 _symmetry_space_group_name_Hall ? 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 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928.00 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator filter _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.58 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -1 -2 -2 0 -2 0 -2 -2 _diffrn_reflns_number 1886 _reflns_number_total 1886 _reflns_number_gt 1467 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.043 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 60.07 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.06429 _diffrn_orient_matrix_UB_12 -0.03388 _diffrn_orient_matrix_UB_13 -0.01581 _diffrn_orient_matrix_UB_21 -0.04466 _diffrn_orient_matrix_UB_22 0.05016 _diffrn_orient_matrix_UB_23 0.01277 _diffrn_orient_matrix_UB_31 0.00485 _diffrn_orient_matrix_UB_32 0.01280 _diffrn_orient_matrix_UB_33 -0.09191 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.031 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.049 0.032 ;International Tables for Crystallography (1992, 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_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.8770(2) 0.5191(2) 0.1553 0.0805(8) Uani 1.00 d . . . O(2) O 0.7553(3) 0.2576(2) -0.1436(4) 0.102(1) Uani 1.00 d . . . O(3) O 0.5778(3) 0.2387(2) -0.1150(6) 0.135(1) Uani 1.00 d . . . O(4) O 0.9401(2) 0.1669(1) 0.3822(4) 0.0656(7) Uani 1.00 d . . . O(5) O 0.8604(3) 0.1660(2) 0.5732(4) 0.0936(10) Uani 1.00 d . . . O(6) O 1.3909(2) 0.4796(2) -0.0371(4) 0.0860(9) Uani 1.00 d . . . N(1) N 0.9708(2) 0.4501(2) 0.3048(4) 0.0592(7) Uani 1.00 d . . . C(1) C 0.8856(3) 0.4638(2) 0.2324(5) 0.0596(8) Uani 1.00 d . . . C(2) C 0.8021(2) 0.4000(2) 0.2676(4) 0.0567(9) Uani 1.00 d . . . C(3) C 0.8669(2) 0.3355(2) 0.3373(4) 0.0515(8) Uani 1.00 d . . . C(4) C 0.8173(3) 0.2757(2) 0.4275(4) 0.0633(10) Uani 1.00 d . . . C(5) C 0.9025(3) 0.2192(2) 0.4782(4) 0.0667(9) Uani 1.00 d . . . C(6) C 0.9963(3) 0.2665(2) 0.5307(5) 0.081(1) Uani 1.00 d . . . C(7) C 1.0403(3) 0.3310(2) 0.4406(5) 0.072(1) Uani 1.00 d . . . C(8) C 0.9517(3) 0.3871(2) 0.4004(4) 0.0581(9) Uani 1.00 d . . . C(9) C 0.7379(2) 0.3648(2) 0.1619(4) 0.0580(8) Uani 1.00 d . . . C(10) C 0.6308(3) 0.3538(3) 0.1779(5) 0.085(1) Uani 1.00 d . . . C(11) C 0.5696(3) 0.3130(3) 0.0878(7) 0.103(2) Uani 1.00 d . . . C(12) C 0.6190(4) 0.2838(3) -0.0158(7) 0.097(1) Uani 1.00 d . . . C(13) C 0.7240(3) 0.2947(2) -0.0330(5) 0.0731(9) Uani 1.00 d . . . C(14) C 0.7856(3) 0.3352(2) 0.0533(4) 0.0636(9) Uani 1.00 d . . . C(15) C 0.6615(6) 0.2346(4) -0.2045(7) 0.136(2) Uani 1.00 d . . . C(16) C 0.8590(4) 0.0843(3) 0.5249(6) 0.090(1) Uani 1.00 d . . . C(17) C 0.8818(4) 0.0932(3) 0.3901(6) 0.083(1) Uani 1.00 d . . . C(18) C 1.0555(3) 0.5103(2) 0.3121(5) 0.0675(10) Uani 1.00 d . . . C(19) C 1.1430(3) 0.4971(2) 0.2179(4) 0.0592(8) Uani 1.00 d . . . C(20) C 1.2263(3) 0.5525(2) 0.2152(5) 0.070(1) Uani 1.00 d . . . C(21) C 1.3062(3) 0.5446(2) 0.1306(5) 0.073(1) Uani 1.00 d . . . C(22) C 1.3074(3) 0.4812(2) 0.0440(5) 0.0655(9) Uani 1.00 d . . . C(23) C 1.2261(3) 0.4261(2) 0.0444(5) 0.074(1) Uani 1.00 d . . . C(24) C 1.1448(3) 0.4338(2) 0.1306(5) 0.070(1) Uani 1.00 d . . . C(25) C 1.3902(4) 0.4185(3) -0.1329(6) 0.097(2) Uani 1.00 d . . . H(1) H 0.7554 0.4251 0.3262 0.0688 Uiso 1.00 calc . . . H(2) H 0.9011 0.3033 0.2749 0.0624 Uiso 1.00 calc . . . H(3) H 0.7857 0.3053 0.4955 0.0755 Uiso 1.00 calc . . . H(4) H 0.7651 0.2441 0.3858 0.0755 Uiso 1.00 calc . . . H(5) H 0.9744 0.2948 0.6053 0.0981 Uiso 1.00 calc . . . H(6) H 1.0500 0.2289 0.5504 0.0981 Uiso 1.00 calc . . . H(7) H 1.0932 0.3631 0.4813 0.0862 Uiso 1.00 calc . . . H(8) H 1.0698 0.3048 0.3689 0.0862 Uiso 1.00 calc . . . H(9) H 0.9223 0.4126 0.4729 0.0701 Uiso 1.00 calc . . . H(10) H 0.5989 0.3739 0.2520 0.1012 Uiso 1.00 calc . . . H(11) H 0.4961 0.3059 0.0979 0.1237 Uiso 1.00 calc . . . H(12) H 0.8591 0.3426 0.0394 0.0772 Uiso 1.00 calc . . . H(13) H 0.6516 0.2690 -0.2759 0.1634 Uiso 1.00 calc . . . H(14) H 0.6717 0.1781 -0.2360 0.1634 Uiso 1.00 calc . . . H(15) H 0.7934 0.0586 0.5374 0.1070 Uiso 1.00 calc . . . H(16) H 0.9127 0.0516 0.5640 0.1070 Uiso 1.00 calc . . . H(17) H 0.8183 0.0975 0.3428 0.0978 Uiso 1.00 calc . . . H(18) H 0.9212 0.0474 0.3589 0.0978 Uiso 1.00 calc . . . H(19) H 1.0268 0.5638 0.2984 0.0815 Uiso 1.00 calc . . . H(20) H 1.0847 0.5077 0.3944 0.0815 Uiso 1.00 calc . . . H(21) H 1.2283 0.5967 0.2736 0.0833 Uiso 1.00 calc . . . H(22) H 1.3622 0.5836 0.1312 0.0880 Uiso 1.00 calc . . . H(23) H 1.2258 0.3816 -0.0139 0.0878 Uiso 1.00 calc . . . H(24) H 1.0889 0.3952 0.1294 0.0847 Uiso 1.00 calc . . . H(25) H 1.3304 0.4260 -0.1853 0.1173 Uiso 1.00 calc . . . H(26) H 1.3894 0.3653 -0.0970 0.1173 Uiso 1.00 calc . . . H(27) H 1.4521 0.4247 -0.1835 0.1173 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(2) 0.062(1) 0.086(2) -0.005(1) -0.017(2) 0.025(1) O(2) 0.165(3) 0.077(2) 0.064(2) -0.014(2) -0.041(2) 0.003(1) O(3) 0.143(3) 0.093(2) 0.170(4) -0.037(2) -0.100(3) 0.005(3) O(4) 0.079(1) 0.060(1) 0.058(1) 0.0013(10) 0.003(1) -0.002(1) O(5) 0.150(3) 0.077(2) 0.054(2) 0.005(2) 0.014(2) 0.018(1) O(6) 0.083(2) 0.088(2) 0.087(2) -0.009(1) 0.016(1) -0.001(1) N(1) 0.064(1) 0.051(1) 0.063(2) 0.000(1) -0.010(1) -0.004(1) C(1) 0.066(2) 0.053(2) 0.060(2) 0.004(1) -0.004(1) -0.002(1) C(2) 0.054(2) 0.060(2) 0.056(2) 0.011(1) -0.003(1) 0.004(1) C(3) 0.054(2) 0.055(2) 0.046(2) 0.009(1) -0.002(1) -0.001(1) C(4) 0.073(2) 0.064(2) 0.053(2) 0.002(1) 0.006(2) 0.004(1) C(5) 0.098(2) 0.054(2) 0.048(2) 0.007(1) -0.009(1) 0.002(1) C(6) 0.107(3) 0.065(2) 0.072(2) 0.011(2) -0.036(2) 0.002(2) C(7) 0.073(2) 0.062(2) 0.080(2) 0.003(1) -0.034(2) -0.010(2) C(8) 0.069(2) 0.056(2) 0.050(2) 0.004(1) -0.010(1) -0.008(1) C(9) 0.055(1) 0.056(2) 0.062(2) 0.004(1) -0.012(1) 0.014(1) C(10) 0.057(1) 0.089(3) 0.109(3) 0.001(2) -0.007(2) 0.032(2) C(11) 0.060(2) 0.100(3) 0.149(4) -0.020(2) -0.034(2) 0.027(3) C(12) 0.089(2) 0.070(2) 0.132(3) -0.011(2) -0.056(2) 0.032(2) C(13) 0.095(2) 0.059(2) 0.064(2) -0.014(2) -0.032(2) 0.023(1) C(14) 0.067(2) 0.066(2) 0.058(2) -0.003(1) -0.012(1) 0.013(1) C(15) 0.196(4) 0.108(4) 0.104(4) -0.062(4) -0.096(3) 0.030(3) C(16) 0.096(3) 0.070(2) 0.105(2) -0.005(2) 0.014(3) 0.019(2) C(17) 0.087(3) 0.063(2) 0.098(2) -0.009(2) -0.004(2) -0.008(2) C(18) 0.074(2) 0.050(2) 0.078(2) -0.007(1) -0.008(2) -0.017(2) C(19) 0.074(2) 0.048(2) 0.056(2) -0.004(1) -0.018(1) 0.004(1) C(20) 0.085(2) 0.054(2) 0.071(2) -0.017(1) -0.012(2) -0.008(2) C(21) 0.082(2) 0.060(2) 0.078(2) -0.022(2) -0.007(2) 0.000(2) C(22) 0.072(2) 0.057(2) 0.067(2) -0.001(1) -0.010(1) 0.007(1) C(23) 0.084(2) 0.060(2) 0.076(2) -0.011(1) -0.003(2) -0.018(2) C(24) 0.074(2) 0.053(2) 0.084(2) -0.017(2) -0.004(2) -0.017(2) C(25) 0.097(3) 0.092(3) 0.103(3) 0.008(2) 0.019(3) -0.019(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00119|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.090(9) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1467 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0584 _refine_ls_wR_factor_gt 0.0584 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.385 _refine_ls_shift/su_max 0.0080 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -0.18 _refine_diff_density_max 0.15 #------------------------------------------------------------------------------ _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) 1.217(5) 1_555 1_555 yes O(2) C(13) 1.377(7) 1_555 1_555 yes O(2) C(15) 1.409(7) 1_555 1_555 yes O(3) C(12) 1.384(8) 1_555 1_555 yes O(3) C(15) 1.43(1) 1_555 1_555 yes O(4) C(5) 1.408(5) 1_555 1_555 yes O(4) C(17) 1.408(6) 1_555 1_555 yes O(5) C(5) 1.431(6) 1_555 1_555 yes O(5) C(16) 1.416(7) 1_555 1_555 yes O(6) C(22) 1.370(6) 1_555 1_555 yes O(6) C(25) 1.418(7) 1_555 1_555 yes N(1) C(1) 1.349(5) 1_555 1_555 yes N(1) C(8) 1.459(5) 1_555 1_555 yes N(1) C(18) 1.457(5) 1_555 1_555 yes C(1) C(2) 1.528(6) 1_555 1_555 yes C(2) C(3) 1.523(5) 1_555 1_555 yes C(2) C(9) 1.502(6) 1_555 1_555 yes C(2) H(1) 0.953 1_555 1_555 no C(3) C(4) 1.502(5) 1_555 1_555 yes C(3) C(8) 1.520(5) 1_555 1_555 yes C(3) H(2) 0.950 1_555 1_555 no C(4) C(5) 1.518(6) 1_555 1_555 yes C(4) H(3) 0.956 1_555 1_555 no C(4) H(4) 0.948 1_555 1_555 no C(5) C(6) 1.525(6) 1_555 1_555 yes C(6) C(7) 1.523(7) 1_555 1_555 yes C(6) H(5) 0.956 1_555 1_555 no C(6) H(6) 0.940 1_555 1_555 no C(7) C(8) 1.509(5) 1_555 1_555 yes C(7) H(7) 0.954 1_555 1_555 no C(7) H(8) 0.950 1_555 1_555 no C(8) H(9) 0.952 1_555 1_555 no C(9) C(10) 1.387(6) 1_555 1_555 yes C(9) C(14) 1.389(6) 1_555 1_555 yes C(10) C(11) 1.400(8) 1_555 1_555 yes C(10) H(10) 0.944 1_555 1_555 no C(11) C(12) 1.353(10) 1_555 1_555 yes C(11) H(11) 0.951 1_555 1_555 no C(12) C(13) 1.362(8) 1_555 1_555 yes C(13) C(14) 1.375(6) 1_555 1_555 yes C(14) H(12) 0.955 1_555 1_555 no C(15) H(13) 0.949 1_555 1_555 no C(15) H(14) 0.981 1_555 1_555 no C(16) C(17) 1.468(8) 1_555 1_555 yes C(16) H(15) 0.943 1_555 1_555 no C(16) H(16) 0.960 1_555 1_555 no C(17) H(17) 0.955 1_555 1_555 no C(17) H(18) 0.953 1_555 1_555 no C(18) C(19) 1.514(7) 1_555 1_555 yes C(18) H(19) 0.950 1_555 1_555 no C(18) H(20) 0.951 1_555 1_555 no C(19) C(20) 1.389(6) 1_555 1_555 yes C(19) C(24) 1.382(6) 1_555 1_555 yes C(20) C(21) 1.365(7) 1_555 1_555 yes C(20) H(21) 0.946 1_555 1_555 no C(21) C(22) 1.378(6) 1_555 1_555 yes C(21) H(22) 0.952 1_555 1_555 no C(22) C(23) 1.365(6) 1_555 1_555 yes C(23) C(24) 1.388(6) 1_555 1_555 yes C(23) H(23) 0.949 1_555 1_555 no C(24) H(24) 0.947 1_555 1_555 no C(25) H(25) 0.951 1_555 1_555 no C(25) H(26) 0.941 1_555 1_555 no C(25) H(27) 0.960 1_555 1_555 no #------------------------------------------------------------------------------ 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) O(2) C(15) 105.1(6) 1_555 1_555 1_555 yes C(12) O(3) C(15) 104.3(4) 1_555 1_555 1_555 yes C(5) O(4) C(17) 106.6(4) 1_555 1_555 1_555 yes C(5) O(5) C(16) 108.0(4) 1_555 1_555 1_555 yes C(22) O(6) C(25) 117.3(4) 1_555 1_555 1_555 yes C(1) N(1) C(8) 112.2(3) 1_555 1_555 1_555 yes C(1) N(1) C(18) 121.1(3) 1_555 1_555 1_555 yes C(8) N(1) C(18) 123.6(3) 1_555 1_555 1_555 yes O(1) C(1) N(1) 125.3(4) 1_555 1_555 1_555 yes O(1) C(1) C(2) 126.6(4) 1_555 1_555 1_555 yes N(1) C(1) C(2) 108.1(3) 1_555 1_555 1_555 yes C(1) C(2) C(3) 101.7(3) 1_555 1_555 1_555 yes C(1) C(2) C(9) 116.9(3) 1_555 1_555 1_555 yes C(1) C(2) H(1) 107.9(4) 1_555 1_555 1_555 no C(3) C(2) C(9) 113.6(3) 1_555 1_555 1_555 yes C(3) C(2) H(1) 108.2(4) 1_555 1_555 1_555 no C(9) C(2) H(1) 108.0(3) 1_555 1_555 1_555 no C(2) C(3) C(4) 121.5(3) 1_555 1_555 1_555 yes C(2) C(3) C(8) 103.0(3) 1_555 1_555 1_555 yes C(2) C(3) H(2) 106.5(4) 1_555 1_555 1_555 no C(4) C(3) C(8) 111.8(3) 1_555 1_555 1_555 yes C(4) C(3) H(2) 106.6(3) 1_555 1_555 1_555 no C(8) C(3) H(2) 106.4(3) 1_555 1_555 1_555 no C(3) C(4) C(5) 108.2(3) 1_555 1_555 1_555 yes C(3) C(4) H(3) 109.6(4) 1_555 1_555 1_555 no C(3) C(4) H(4) 110.1(4) 1_555 1_555 1_555 no C(5) C(4) H(3) 109.6(4) 1_555 1_555 1_555 no C(5) C(4) H(4) 110.2(4) 1_555 1_555 1_555 no H(3) C(4) H(4) 109.1(4) 1_555 1_555 1_555 no O(4) C(5) O(5) 106.1(3) 1_555 1_555 1_555 yes O(4) C(5) C(4) 110.3(3) 1_555 1_555 1_555 yes O(4) C(5) C(6) 107.4(4) 1_555 1_555 1_555 yes O(5) C(5) C(4) 110.1(4) 1_555 1_555 1_555 yes O(5) C(5) C(6) 109.7(4) 1_555 1_555 1_555 yes C(4) C(5) C(6) 112.9(3) 1_555 1_555 1_555 yes C(5) C(6) C(7) 113.7(4) 1_555 1_555 1_555 yes C(5) C(6) H(5) 108.3(5) 1_555 1_555 1_555 no C(5) C(6) H(6) 109.1(4) 1_555 1_555 1_555 no C(7) C(6) H(5) 107.5(4) 1_555 1_555 1_555 no C(7) C(6) H(6) 108.4(5) 1_555 1_555 1_555 no H(5) C(6) H(6) 109.8(6) 1_555 1_555 1_555 no C(6) C(7) C(8) 108.2(4) 1_555 1_555 1_555 yes C(6) C(7) H(7) 110.3(5) 1_555 1_555 1_555 no C(6) C(7) H(8) 110.1(4) 1_555 1_555 1_555 no C(8) C(7) H(7) 109.3(3) 1_555 1_555 1_555 no C(8) C(7) H(8) 109.7(4) 1_555 1_555 1_555 no H(7) C(7) H(8) 109.1(5) 1_555 1_555 1_555 no N(1) C(8) C(3) 101.2(3) 1_555 1_555 1_555 yes N(1) C(8) C(7) 119.4(4) 1_555 1_555 1_555 yes N(1) C(8) H(9) 109.1(3) 1_555 1_555 1_555 no C(3) C(8) C(7) 109.2(3) 1_555 1_555 1_555 yes C(3) C(8) H(9) 108.3(4) 1_555 1_555 1_555 no C(7) C(8) H(9) 109.1(4) 1_555 1_555 1_555 no C(2) C(9) C(10) 119.6(4) 1_555 1_555 1_555 yes C(2) C(9) C(14) 120.8(3) 1_555 1_555 1_555 yes C(10) C(9) C(14) 119.3(4) 1_555 1_555 1_555 yes C(9) C(10) C(11) 121.7(5) 1_555 1_555 1_555 yes C(9) C(10) H(10) 118.8(5) 1_555 1_555 1_555 no C(11) C(10) H(10) 119.5(5) 1_555 1_555 1_555 no C(10) C(11) C(12) 117.5(5) 1_555 1_555 1_555 yes C(10) C(11) H(11) 121.9(8) 1_555 1_555 1_555 no C(12) C(11) H(11) 120.6(7) 1_555 1_555 1_555 no O(3) C(12) C(11) 128.7(6) 1_555 1_555 1_555 yes O(3) C(12) C(13) 109.8(7) 1_555 1_555 1_555 yes C(11) C(12) C(13) 121.4(6) 1_555 1_555 1_555 yes O(2) C(13) C(12) 110.1(5) 1_555 1_555 1_555 yes O(2) C(13) C(14) 127.7(5) 1_555 1_555 1_555 yes C(12) C(13) C(14) 122.2(5) 1_555 1_555 1_555 yes C(9) C(14) C(13) 117.9(4) 1_555 1_555 1_555 yes C(9) C(14) H(12) 121.0(4) 1_555 1_555 1_555 no C(13) C(14) H(12) 121.1(5) 1_555 1_555 1_555 no O(2) C(15) O(3) 108.4(5) 1_555 1_555 1_555 yes O(2) C(15) H(13) 108.9(6) 1_555 1_555 1_555 no O(2) C(15) H(14) 106.9(8) 1_555 1_555 1_555 no O(3) C(15) H(13) 113.9(9) 1_555 1_555 1_555 no O(3) C(15) H(14) 111.6(7) 1_555 1_555 1_555 no H(13) C(15) H(14) 106.9(9) 1_555 1_555 1_555 no O(5) C(16) C(17) 105.1(4) 1_555 1_555 1_555 yes O(5) C(16) H(15) 111.8(5) 1_555 1_555 1_555 no O(5) C(16) H(16) 110.3(6) 1_555 1_555 1_555 no C(17) C(16) H(15) 110.9(6) 1_555 1_555 1_555 no C(17) C(16) H(16) 109.6(6) 1_555 1_555 1_555 no H(15) C(16) H(16) 109.2(5) 1_555 1_555 1_555 no O(4) C(17) C(16) 104.2(4) 1_555 1_555 1_555 yes O(4) C(17) H(17) 110.7(5) 1_555 1_555 1_555 no O(4) C(17) H(18) 111.0(5) 1_555 1_555 1_555 no C(16) C(17) H(17) 110.6(6) 1_555 1_555 1_555 no C(16) C(17) H(18) 111.6(6) 1_555 1_555 1_555 no H(17) C(17) H(18) 108.7(6) 1_555 1_555 1_555 no N(1) C(18) C(19) 114.6(3) 1_555 1_555 1_555 yes N(1) C(18) H(19) 108.3(4) 1_555 1_555 1_555 no N(1) C(18) H(20) 108.0(4) 1_555 1_555 1_555 no C(19) C(18) H(19) 108.2(4) 1_555 1_555 1_555 no C(19) C(18) H(20) 108.2(4) 1_555 1_555 1_555 no H(19) C(18) H(20) 109.4(4) 1_555 1_555 1_555 no C(18) C(19) C(20) 119.0(4) 1_555 1_555 1_555 yes C(18) C(19) C(24) 124.1(4) 1_555 1_555 1_555 yes C(20) C(19) C(24) 116.8(4) 1_555 1_555 1_555 yes C(19) C(20) C(21) 121.6(4) 1_555 1_555 1_555 yes C(19) C(20) H(21) 119.6(5) 1_555 1_555 1_555 no C(21) C(20) H(21) 118.8(4) 1_555 1_555 1_555 no C(20) C(21) C(22) 121.2(4) 1_555 1_555 1_555 yes C(20) C(21) H(22) 119.6(5) 1_555 1_555 1_555 no C(22) C(21) H(22) 119.3(5) 1_555 1_555 1_555 no O(6) C(22) C(21) 116.2(4) 1_555 1_555 1_555 yes O(6) C(22) C(23) 125.5(4) 1_555 1_555 1_555 yes C(21) C(22) C(23) 118.3(4) 1_555 1_555 1_555 yes C(22) C(23) C(24) 120.7(4) 1_555 1_555 1_555 yes C(22) C(23) H(23) 119.6(5) 1_555 1_555 1_555 no C(24) C(23) H(23) 119.6(4) 1_555 1_555 1_555 no C(19) C(24) C(23) 121.4(4) 1_555 1_555 1_555 yes C(19) C(24) H(24) 118.9(5) 1_555 1_555 1_555 no C(23) C(24) H(24) 119.6(4) 1_555 1_555 1_555 no O(6) C(25) H(25) 109.7(5) 1_555 1_555 1_555 no O(6) C(25) H(26) 110.2(6) 1_555 1_555 1_555 no O(6) C(25) H(27) 108.9(5) 1_555 1_555 1_555 no H(25) C(25) H(26) 110.1(6) 1_555 1_555 1_555 no H(25) C(25) H(27) 108.5(8) 1_555 1_555 1_555 no H(26) C(25) H(27) 109.4(6) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(1) C(1) N(1) C(8) 171.6(4) 1_555 1_555 1_555 1_555 yes O(1) C(1) N(1) C(18) 10.8(7) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(2) C(3) 164.8(4) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(2) C(9) 40.4(6) 1_555 1_555 1_555 1_555 yes O(2) C(13) C(12) O(3) 0.2(5) 1_555 1_555 1_555 1_555 yes O(2) C(13) C(12) C(11) 178.5(5) 1_555 1_555 1_555 1_555 yes O(2) C(13) C(14) C(9) -177.1(4) 1_555 1_555 1_555 1_555 yes O(2) C(15) O(3) C(12) 15.0(7) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(11) C(10) 177.0(5) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(14) -178.0(4) 1_555 1_555 1_555 1_555 yes O(3) C(15) O(2) C(13) -14.9(6) 1_555 1_555 1_555 1_555 yes O(4) C(5) O(5) C(16) -8.7(5) 1_555 1_555 1_555 1_555 yes O(4) C(5) C(4) C(3) -68.5(4) 1_555 1_555 1_555 1_555 yes O(4) C(5) C(6) C(7) 70.6(4) 1_555 1_555 1_555 1_555 yes O(4) C(17) C(16) O(5) 26.4(6) 1_555 1_555 1_555 1_555 yes O(5) C(5) O(4) C(17) 25.8(5) 1_555 1_555 1_555 1_555 yes O(5) C(5) C(4) C(3) 174.7(3) 1_555 1_555 1_555 1_555 yes O(5) C(5) C(6) C(7) -174.4(4) 1_555 1_555 1_555 1_555 yes O(6) C(22) C(21) C(20) 179.4(4) 1_555 1_555 1_555 1_555 yes O(6) C(22) C(23) C(24) -179.6(4) 1_555 1_555 1_555 1_555 yes N(1) C(1) C(2) C(3) -17.0(4) 1_555 1_555 1_555 1_555 yes N(1) C(1) C(2) C(9) -141.3(3) 1_555 1_555 1_555 1_555 yes N(1) C(8) C(3) C(2) -36.3(4) 1_555 1_555 1_555 1_555 yes N(1) C(8) C(3) C(4) -168.5(3) 1_555 1_555 1_555 1_555 yes N(1) C(8) C(7) C(6) -174.5(3) 1_555 1_555 1_555 1_555 yes N(1) C(18) C(19) C(20) 178.4(4) 1_555 1_555 1_555 1_555 yes N(1) C(18) C(19) C(24) 0.2(6) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(8) C(3) 27.4(4) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(8) C(7) 147.1(3) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(18) C(19) -91.9(5) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 158.8(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(8) 32.7(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(9) C(10) -138.3(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(9) C(14) 48.4(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) N(1) C(8) -6.6(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) N(1) C(18) -167.4(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 178.8(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(8) C(7) -163.1(3) 1_555 1_555 1_555 1_555 yes C(2) C(9) C(10) C(11) -172.9(4) 1_555 1_555 1_555 1_555 yes C(2) C(9) C(14) C(13) 172.2(3) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(9) C(10) 103.7(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(9) C(14) -69.6(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 51.8(5) 1_555 1_555 1_555 1_555 yes C(3) C(8) N(1) C(18) -172.4(3) 1_555 1_555 1_555 1_555 yes C(3) C(8) C(7) C(6) -58.9(4) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(9) -74.7(5) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(8) C(7) 64.8(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) O(4) C(17) -93.4(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) O(5) C(16) 110.7(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) -51.3(5) 1_555 1_555 1_555 1_555 yes C(5) O(4) C(17) C(16) -32.3(5) 1_555 1_555 1_555 1_555 yes C(5) O(5) C(16) C(17) -10.9(6) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(3) C(8) -59.1(4) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 53.7(5) 1_555 1_555 1_555 1_555 yes C(6) C(5) O(4) C(17) 143.1(4) 1_555 1_555 1_555 1_555 yes C(6) C(5) O(5) C(16) -124.4(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) N(1) C(18) -52.7(5) 1_555 1_555 1_555 1_555 yes C(8) N(1) C(18) C(19) 109.6(4) 1_555 1_555 1_555 1_555 yes C(8) C(3) C(2) C(9) 159.2(3) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(12) 0.6(8) 1_555 1_555 1_555 1_555 yes C(9) C(14) C(13) C(12) 0.8(6) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(14) C(13) -1.2(6) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(12) C(13) -1.0(8) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(9) C(14) 0.5(7) 1_555 1_555 1_555 1_555 yes C(11) C(12) O(3) C(15) 172.5(6) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 0.3(7) 1_555 1_555 1_555 1_555 yes C(12) C(13) O(2) C(15) 9.2(5) 1_555 1_555 1_555 1_555 yes C(13) C(12) O(3) C(15) -9.3(6) 1_555 1_555 1_555 1_555 yes C(14) C(13) O(2) C(15) -172.7(4) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(21) -178.6(4) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(24) C(23) 178.3(4) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(21) C(22) 0.2(7) 1_555 1_555 1_555 1_555 yes C(19) C(24) C(23) C(22) 0.2(7) 1_555 1_555 1_555 1_555 yes C(20) C(19) C(24) C(23) 0.1(7) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(23) 0.1(7) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(19) C(24) -0.3(7) 1_555 1_555 1_555 1_555 yes C(21) C(22) O(6) C(25) -175.7(5) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) -0.3(7) 1_555 1_555 1_555 1_555 yes C(23) C(22) O(6) C(25) 3.6(7) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(16) 3.476(6) 1_555 3_654 ? O(1) C(7) 3.490(5) 1_555 2_764 ? O(2) C(25) 3.329(8) 1_555 4_455 ? O(2) C(20) 3.424(5) 1_555 2_764 ? O(2) C(23) 3.599(6) 1_555 4_455 ? O(4) C(10) 3.277(6) 1_555 4_555 ? O(4) C(11) 3.553(9) 1_555 4_555 ? O(5) C(25) 3.429(7) 1_555 4_456 ? O(6) C(17) 3.516(6) 1_555 3_754 ? C(6) C(15) 3.514(7) 1_555 4_556 ? C(17) C(20) 3.596(7) 1_555 4_455 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ;