Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_3H-azepine_photodimer _database_code_CSD 158836 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Kimura, Masaru' 'Satake, Kyosuke' 'Takami, Shizuka' 'Tawada, Yuko' _publ_contact_author_name 'Dr Kyosuke Satake' _publ_contact_author_address ; Dr Kyosuke Satake Department of Chemistry Okayama University Faculty of Science Tsushima-Naka 3-1-1 Okayama 700-8530 JAPAN ; _publ_contact_author_email 'SATAKE@CC.OKAYAMA-U.AC.JP' _publ_section_title ; Photochemical Behaviour of 2,5-Di-tert-butyl-3H-azepine: Unexpected Formation of a Dicyclopenta[b,e]pyridine Derivative and a cis,cis-Cyclodeca-1,6-diene Derivative ; #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan for Windows version 1.06' _computing_publication_material 'teXsan for Windows version 1.06' #------------------------------------------------------------------------------ _cell_length_a 11.400(2) _cell_length_b 21.835(6) _cell_length_c 10.935(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2721.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 11.1 _cell_measurement_theta_max 11.5 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plates' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 429.68 _chemical_formula_analytical ? _chemical_formula_sum 'C28 H47 N O2 ' _chemical_formula_moiety 'C28 H47 N O2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type ; psi-scan (North, Phillips & Mathews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.947 _exptl_special_details ; The scan width was (1.73+0.30tan\q)\% with an \w scan speed of 6\% per minute (up to 2 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 3.92 _diffrn_reflns_number 3138 _reflns_number_total 2743 _reflns_number_gt 1468 _reflns_threshold_expression I>2\s(I) _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.080 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 25.95 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.06821 _diffrn_orient_matrix_UB_12 -0.01780 _diffrn_orient_matrix_UB_13 0.04530 _diffrn_orient_matrix_UB_21 -0.03314 _diffrn_orient_matrix_UB_22 0.04204 _diffrn_orient_matrix_UB_23 0.01160 _diffrn_orient_matrix_UB_31 -0.04410 _diffrn_orient_matrix_UB_32 -0.00404 _diffrn_orient_matrix_UB_33 -0.07878 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 112 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 188 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 8 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom O1 0.6343(5) -0.0039(3) 0.3836(5) 0.0498(16) 1.000 . Uani d ? O2 0.8959(6) 0.1064(3) 0.7268(6) 0.072(2) 1.000 . Uani d ? N1 0.5788(5) 0.0689(3) 0.5926(6) 0.0383(17) 1.000 . Uani d ? C2 0.6903(7) 0.0383(3) 0.6233(7) 0.0358(19) 1.000 . Uani d ? C3 0.6947(6) -0.0303(3) 0.5889(7) 0.0360(19) 1.000 . Uani d ? C4 0.6075(6) -0.0429(3) 0.4844(7) 0.0362(19) 1.000 . Uani d ? C5 0.4810(6) -0.0316(4) 0.5311(8) 0.043(2) 1.000 . Uani d ? C6 0.4748(7) 0.0298(4) 0.6063(7) 0.044(2) 1.000 . Uani d ? C7 0.4365(7) -0.0797(4) 0.6159(8) 0.048(2) 1.000 . Uani d ? C8 0.4243(7) -0.0585(4) 0.7276(8) 0.052(3) 1.000 . Uani d ? C9 0.4597(7) 0.0083(4) 0.7400(8) 0.050(2) 1.000 . Uani d ? C10 0.8243(6) -0.0405(4) 0.5608(7) 0.041(2) 1.000 . Uani d ? C11 0.8765(6) 0.0122(4) 0.5455(8) 0.044(2) 1.000 . Uani d ? C12 0.7954(6) 0.0676(3) 0.5561(7) 0.0349(18) 1.000 . Uani d ? C13 0.8803(7) -0.1040(4) 0.5590(8) 0.048(2) 1.000 . Uani d ? C14 0.8494(8) -0.1378(4) 0.4446(10) 0.062(3) 1.000 . Uani d ? C15 0.8448(10) -0.1409(5) 0.6703(10) 0.076(3) 1.000 . Uani d ? C16 1.0136(8) -0.0973(5) 0.5627(12) 0.074(3) 1.000 . Uani d ? C17 0.4031(7) -0.1451(4) 0.5739(9) 0.053(2) 1.000 . Uani d ? C18 0.3476(11) -0.1430(5) 0.4477(12) 0.087(4) 1.000 . Uani d ? C19 0.3145(9) -0.1738(5) 0.6634(11) 0.074(3) 1.000 . Uani d ? C20 0.5119(9) -0.1860(4) 0.5696(15) 0.095(4) 1.000 . Uani d ? C21 0.3649(7) 0.0693(4) 0.5659(9) 0.052(2) 1.000 . Uani d ? C22 0.3590(10) 0.1285(5) 0.6449(12) 0.084(4) 1.000 . Uani d ? C23 0.2501(7) 0.0367(5) 0.5804(11) 0.071(3) 1.000 . Uani d ? C24 0.3767(10) 0.0910(4) 0.4326(10) 0.074(3) 1.000 . Uani d ? C25 0.8542(8) 0.1184(4) 0.6290(7) 0.046(2) 1.000 . Uani d ? C26 0.8625(8) 0.1825(3) 0.5752(8) 0.050(2) 1.000 . Uani d ? C27 0.7419(11) 0.2053(6) 0.5454(13) 0.093(4) 1.000 . Uani d ? C28 0.9211(13) 0.2247(5) 0.6682(12) 0.105(5) 1.000 . Uani d ? C29 0.9383(12) 0.1785(6) 0.4608(12) 0.098(4) 1.000 . Uani d ? H1O 0.625(10) -0.021(5) 0.307(11) 0.11(4) 1.000 . Uiso d ? H1N 0.591(6) 0.084(3) 0.502(7) 0.035(19) 1.000 . Uiso d ? H2 0.7017 0.0419 0.7112 0.045 1.000 . Uiso c ? H3 0.6739 -0.0552 0.6564 0.047 1.000 . Uiso c ? H4 0.6146 -0.0847 0.4586 0.046 1.000 . Uiso c ? H5 0.4293 -0.0294 0.4629 0.056 1.000 . Uiso c ? H8 0.3943 -0.0807 0.7958 0.063 1.000 . Uiso c ? H11 0.9586 0.0173 0.5270 0.057 1.000 . Uiso c ? H12 0.7717 0.0821 0.4761 0.051 1.000 . Uiso c ? H91 0.5319 0.0111 0.7832 0.065 1.000 . Uiso c ? H92 0.4013 0.0310 0.7817 0.065 1.000 . Uiso c ? H141 0.7973 -0.1127 0.3942 0.089 1.000 . Uiso c ? H142 0.9167 -0.1467 0.3970 0.089 1.000 . Uiso c ? H143 0.8088 -0.1744 0.4634 0.089 1.000 . Uiso c ? H151 0.8822 -0.1793 0.6690 0.083 1.000 . Uiso c ? H152 0.7621 -0.1460 0.6705 0.083 1.000 . Uiso c ? H153 0.8670 -0.1193 0.7435 0.083 1.000 . Uiso c ? H161 1.0494 -0.1324 0.5257 0.098 1.000 . Uiso c ? H162 1.0388 -0.0983 0.6496 0.098 1.000 . Uiso c ? H163 1.0402 -0.0615 0.5282 0.098 1.000 . Uiso c ? H181 0.2653 -0.1378 0.4572 0.108 1.000 . Uiso c ? H182 0.3646 -0.1796 0.4076 0.108 1.000 . Uiso c ? H183 0.3793 -0.1089 0.4055 0.108 1.000 . Uiso c ? H191 0.2383 -0.1641 0.6398 0.090 1.000 . Uiso c ? H192 0.3266 -0.2168 0.6643 0.090 1.000 . Uiso c ? H193 0.3299 -0.1580 0.7440 0.090 1.000 . Uiso c ? H201 0.5200 -0.2059 0.6452 0.116 1.000 . Uiso c ? H202 0.4999 -0.2150 0.5060 0.116 1.000 . Uiso c ? H203 0.5771 -0.1612 0.5522 0.116 1.000 . Uiso c ? H221 0.4227 0.1532 0.6341 0.107 1.000 . Uiso c ? H222 0.2869 0.1486 0.6321 0.107 1.000 . Uiso c ? H223 0.3580 0.1146 0.7324 0.107 1.000 . Uiso c ? H231 0.2450 0.0037 0.5206 0.087 1.000 . Uiso c ? H232 0.1865 0.0631 0.5688 0.087 1.000 . Uiso c ? H233 0.2458 0.0181 0.6595 0.087 1.000 . Uiso c ? H241 0.4412 0.1183 0.4271 0.092 1.000 . Uiso c ? H242 0.3062 0.1132 0.4127 0.092 1.000 . Uiso c ? H243 0.3856 0.0576 0.3815 0.092 1.000 . Uiso c ? H271 0.7496 0.2469 0.5215 0.123 1.000 . Uiso c ? H272 0.7116 0.1814 0.4833 0.123 1.000 . Uiso c ? H273 0.6966 0.2027 0.6177 0.123 1.000 . Uiso c ? H281 0.8918 0.2642 0.6606 0.125 1.000 . Uiso c ? H282 1.0040 0.2241 0.6551 0.125 1.000 . Uiso c ? H283 0.9060 0.2091 0.7488 0.125 1.000 . Uiso c ? H291 0.9233 0.2150 0.4121 0.117 1.000 . Uiso c ? H292 1.0168 0.1762 0.4801 0.117 1.000 . Uiso c ? H293 0.9136 0.1441 0.4135 0.117 1.000 . Uiso c ? 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 O1 0.054(3) 0.062(3) 0.034(3) -0.013(3) 0.008(3) 0.002(3) O2 0.101(5) 0.059(4) 0.057(4) -0.039(4) -0.022(4) 0.016(3) N1 0.035(3) 0.030(3) 0.050(4) 0.003(3) -0.002(3) 0.013(3) C2 0.040(4) 0.034(4) 0.034(4) -0.012(3) -0.001(3) -0.009(3) C3 0.031(4) 0.035(4) 0.042(4) 0.003(3) -0.001(3) -0.001(3) C4 0.036(4) 0.029(3) 0.044(4) -0.006(3) 0.005(3) -0.007(3) C5 0.026(3) 0.049(4) 0.055(5) -0.017(3) -0.003(4) -0.005(4) C6 0.035(4) 0.055(5) 0.041(4) -0.002(4) 0.004(4) 0.012(4) C7 0.035(4) 0.054(5) 0.054(5) -0.005(4) 0.005(4) -0.003(4) C8 0.038(4) 0.060(5) 0.060(6) -0.008(4) 0.009(4) 0.002(5) C9 0.045(5) 0.060(5) 0.045(5) 0.002(4) 0.006(4) -0.005(4) C10 0.031(4) 0.048(4) 0.043(4) 0.000(3) 0.013(3) -0.012(4) C11 0.028(4) 0.046(5) 0.058(5) -0.004(3) 0.000(4) -0.010(4) C12 0.036(4) 0.034(4) 0.034(4) 0.000(3) 0.006(3) 0.006(3) C13 0.045(5) 0.041(4) 0.057(5) 0.006(4) -0.006(4) -0.002(4) C14 0.059(6) 0.046(5) 0.082(7) 0.016(4) -0.008(6) -0.012(5) C15 0.085(8) 0.053(6) 0.090(8) 0.018(6) 0.010(7) 0.026(6) C16 0.042(5) 0.066(6) 0.114(9) 0.018(5) -0.013(6) -0.003(7) C17 0.036(4) 0.057(5) 0.065(6) -0.013(4) -0.000(4) 0.009(5) C18 0.103(9) 0.069(6) 0.089(8) -0.042(7) 0.000(8) -0.018(6) C19 0.062(6) 0.068(6) 0.092(8) -0.028(5) 0.015(6) 0.001(6) C20 0.064(6) 0.042(5) 0.178(13) -0.007(5) 0.026(8) -0.019(7) C21 0.046(4) 0.044(4) 0.067(6) 0.012(4) 0.004(5) 0.008(4) C22 0.063(6) 0.080(7) 0.111(9) 0.021(6) 0.012(7) 0.005(7) C23 0.036(4) 0.086(7) 0.089(7) 0.006(5) -0.004(5) 0.017(7) C24 0.077(7) 0.056(5) 0.088(7) 0.007(5) -0.034(6) 0.033(5) C25 0.048(5) 0.049(5) 0.039(5) -0.010(4) 0.002(4) 0.007(4) C26 0.063(5) 0.029(4) 0.060(5) -0.007(4) 0.003(5) 0.008(4) C27 0.090(8) 0.075(7) 0.113(10) 0.017(7) -0.014(8) -0.002(7) C28 0.149(12) 0.044(5) 0.124(10) -0.022(7) -0.041(10) -0.024(6) C29 0.115(10) 0.082(8) 0.098(9) -0.017(8) 0.044(8) 0.022(7) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.010|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'not determined' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2693 _refine_ls_number_parameters 288 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.164 _refine_ls_R_factor_gt 0.089 _refine_ls_wR_factor_all 0.178 _refine_ls_wR_factor_ref 0.178 _refine_ls_goodness_of_fit_all 1.149 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0005 _refine_diff_density_min -0.29 _refine_diff_density_max 0.41 #============================================================================== # MOLECULAR GEOMETRY _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 O1 C4 1.424(10) . . ? O1 H1O 0.92(12) . . no O2 C25 1.199(10) . . ? N1 C2 1.473(10) . . ? N1 C6 1.469(10) . . ? N1 H1N 1.05(8) . . no C2 C3 1.547(11) . . ? C2 C12 1.544(11) . . ? C2 H2 0.97 . . no C3 C4 1.540(11) . . ? C3 C10 1.525(11) . . ? C3 H3 0.95 . . no C4 C5 1.549(11) . . ? C4 H4 0.96 . . no C5 C6 1.575(12) . . ? C5 C7 1.490(12) . . ? C5 H5 0.95 . . no C6 C9 1.545(12) . . ? C6 C21 1.584(12) . . ? C7 C8 1.313(14) . . ? C7 C17 1.549(12) . . ? C8 C9 1.521(13) . . ? C8 H8 0.95 . . no C9 H91 0.95 . . no C9 H92 0.95 . . no C10 C11 1.306(12) . . ? C10 C13 1.528(12) . . ? C11 C12 1.527(11) . . ? C11 H11 0.96 . . no C12 C25 1.523(11) . . ? C12 H12 0.97 . . no C13 C14 1.495(14) . . ? C13 C15 1.514(14) . . ? C13 C16 1.527(13) . . ? C14 H141 0.98 . . no C14 H142 0.95 . . no C14 H143 0.95 . . no C15 H151 0.94 . . no C15 H152 0.95 . . no C15 H153 0.96 . . no C16 H161 0.96 . . no C16 H162 0.99 . . no C16 H163 0.92 . . no C17 C18 1.519(16) . . ? C17 C19 1.539(14) . . ? C17 C20 1.529(14) . . ? C18 H181 0.95 . . no C18 H182 0.93 . . no C18 H183 0.95 . . no C19 H191 0.93 . . no C19 H192 0.95 . . no C19 H193 0.96 . . no C20 H201 0.94 . . no C20 H202 0.95 . . no C20 H203 0.94 . . no C21 C22 1.557(15) . . ? C21 C23 1.498(13) . . ? C21 C24 1.539(15) . . ? C22 H221 0.91 . . no C22 H222 0.94 . . no C22 H223 1.00 . . no C23 H231 0.98 . . no C23 H232 0.93 . . no C23 H233 0.96 . . no C24 H241 0.95 . . no C24 H242 0.96 . . no C24 H243 0.92 . . no C25 C26 1.520(11) . . ? C26 C27 1.498(15) . . ? C26 C28 1.526(15) . . ? C26 C29 1.523(15) . . ? C27 H271 0.95 . . no C27 H272 0.92 . . no C27 H273 0.95 . . no C28 H281 0.93 . . no C28 H282 0.96 . . no C28 H283 0.96 . . no C29 H291 0.97 . . no C29 H292 0.92 . . no C29 H293 0.95 . . 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 C4 O1 H1O 116(8) . . . no C2 N1 C6 114.2(6) . . . ? C2 N1 H1N 104(4) . . . no C6 N1 H1N 113(4) . . . no N1 C2 C3 114.3(6) . . . ? N1 C2 C12 111.9(6) . . . ? N1 C2 H2 108 . . . no C3 C2 C12 105.0(6) . . . ? C3 C2 H2 108 . . . no C12 C2 H2 109 . . . no C2 C3 C4 109.4(6) . . . ? C2 C3 C10 102.8(6) . . . ? C2 C3 H3 111 . . . no C4 C3 C10 116.7(7) . . . ? C4 C3 H3 108 . . . no C10 C3 H3 109 . . . no O1 C4 C3 109.3(6) . . . ? O1 C4 C5 111.1(7) . . . ? O1 C4 H4 109 . . . no C3 C4 C5 109.1(6) . . . ? C3 C4 H4 110 . . . no C5 C4 H4 109 . . . no C4 C5 C6 110.4(6) . . . ? C4 C5 C7 114.2(7) . . . ? C4 C5 H5 109 . . . no C6 C5 C7 105.1(7) . . . ? C6 C5 H5 110 . . . no C7 C5 H5 108 . . . no N1 C6 C5 113.9(6) . . . ? N1 C6 C9 111.3(7) . . . ? N1 C6 C21 107.1(7) . . . ? C5 C6 C9 103.9(7) . . . ? C5 C6 C21 110.7(7) . . . ? C9 C6 C21 109.9(7) . . . ? C5 C7 C8 111.5(8) . . . ? C5 C7 C17 123.3(8) . . . ? C8 C7 C17 125.1(9) . . . ? C7 C8 C9 113.2(8) . . . ? C7 C8 H8 126 . . . no C9 C8 H8 121 . . . no C6 C9 C8 103.7(7) . . . ? C6 C9 H91 111 . . . no C6 C9 H92 112 . . . no C8 C9 H91 110 . . . no C8 C9 H92 111 . . . no H91 C9 H92 110 . . . no C3 C10 C11 109.9(7) . . . ? C3 C10 C13 122.6(7) . . . ? C11 C10 C13 127.4(7) . . . ? C10 C11 C12 114.3(7) . . . ? C10 C11 H11 125 . . . no C12 C11 H11 121 . . . no C2 C12 C11 100.3(6) . . . ? C2 C12 C25 113.2(7) . . . ? C2 C12 H12 110 . . . no C11 C12 C25 110.5(7) . . . ? C11 C12 H12 111 . . . no C25 C12 H12 111 . . . no C10 C13 C14 111.1(7) . . . ? C10 C13 C15 111.2(8) . . . ? C10 C13 C16 109.2(8) . . . ? C14 C13 C15 110.4(8) . . . ? C14 C13 C16 107.7(9) . . . ? C15 C13 C16 107.2(9) . . . ? C13 C14 H141 110 . . . no C13 C14 H142 112 . . . no C13 C14 H143 111 . . . no H141 C14 H142 107 . . . no H141 C14 H143 107 . . . no H142 C14 H143 110 . . . no C13 C15 H151 110 . . . no C13 C15 H152 109 . . . no C13 C15 H153 110 . . . no H151 C15 H152 110 . . . no H151 C15 H153 109 . . . no H152 C15 H153 108 . . . no C13 C16 H161 110 . . . no C13 C16 H162 108 . . . no C13 C16 H163 114 . . . no H161 C16 H162 105 . . . no H161 C16 H163 112 . . . no H162 C16 H163 108 . . . no C7 C17 C18 110.1(8) . . . ? C7 C17 C19 110.3(8) . . . ? C7 C17 C20 110.3(7) . . . ? C18 C17 C19 108.5(8) . . . ? C18 C17 C20 109.2(11) . . . ? C19 C17 C20 108.4(9) . . . ? C17 C18 H181 108 . . . no C17 C18 H182 108 . . . no C17 C18 H183 108 . . . no H181 C18 H182 111 . . . no H181 C18 H183 110 . . . no H182 C18 H183 111 . . . no C17 C19 H191 110 . . . no C17 C19 H192 108 . . . no C17 C19 H193 109 . . . no H191 C19 H192 111 . . . no H191 C19 H193 110 . . . no H192 C19 H193 109 . . . no C17 C20 H201 109 . . . no C17 C20 H202 107 . . . no C17 C20 H203 108 . . . no H201 C20 H202 111 . . . no H201 C20 H203 112 . . . no H202 C20 H203 111 . . . no C6 C21 C22 109.4(9) . . . ? C6 C21 C23 113.8(7) . . . ? C6 C21 C24 111.3(8) . . . ? C22 C21 C23 107.3(9) . . . ? C22 C21 C24 105.9(8) . . . ? C23 C21 C24 108.8(9) . . . ? C21 C22 H221 113 . . . no C21 C22 H222 110 . . . no C21 C22 H223 106 . . . no H221 C22 H222 114 . . . no H221 C22 H223 108 . . . no H222 C22 H223 106 . . . no C21 C23 H231 109 . . . no C21 C23 H232 112 . . . no C21 C23 H233 110 . . . no H231 C23 H232 109 . . . no H231 C23 H233 107 . . . no H232 C23 H233 110 . . . no C21 C24 H241 109 . . . no C21 C24 H242 107 . . . no C21 C24 H243 110 . . . no H241 C24 H242 108 . . . no H241 C24 H243 112 . . . no H242 C24 H243 111 . . . no O2 C25 C12 118.8(8) . . . ? O2 C25 C26 121.5(8) . . . ? C12 C25 C26 119.7(8) . . . ? C25 C26 C27 109.4(8) . . . ? C25 C26 C28 109.0(8) . . . ? C25 C26 C29 107.4(8) . . . ? C27 C26 C28 110.2(10) . . . ? C27 C26 C29 111.2(10) . . . ? C28 C26 C29 109.5(10) . . . ? C26 C27 H271 107 . . . no C26 C27 H272 108 . . . no C26 C27 H273 107 . . . no H271 C27 H272 112 . . . no H271 C27 H273 110 . . . no H272 C27 H273 112 . . . no C26 C28 H281 110 . . . no C26 C28 H282 109 . . . no C26 C28 H283 109 . . . no H281 C28 H282 111 . . . no H281 C28 H283 110 . . . no H282 C28 H283 108 . . . no C26 C29 H291 108 . . . no C26 C29 H292 112 . . . no C26 C29 H293 109 . . . no H291 C29 H292 110 . . . no H291 C29 H293 107 . . . no H292 C29 H293 112 . . . no #------------------------------------------------------------------------------ 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 O2 C4 3.140(10) . 2_655 no C2 H1O 2.94(13) . 2_655 no C11 H1O 2.87(13) . 2_655 no C25 H1O 2.89(13) . 2_655 no H1O H2 2.2828 . 2_654 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1 C4 C3 C2 . . . . 56.4(8) no O1 C4 C3 C10 . . . . -59.7(9) no O1 C4 C5 C6 . . . . -75.4(8) no O1 C4 C5 C7 . . . . 166.4(7) no O2 C25 C12 C2 . . . . 60.4(11) no O2 C25 C12 C11 . . . . -51.2(11) no O2 C25 C26 C27 . . . . -124.6(12) no O2 C25 C26 C28 . . . . -3.9(14) no O2 C25 C26 C29 . . . . 114.6(11) no N1 C2 C3 C4 . . . . 24.6(9) no N1 C2 C3 C10 . . . . 149.2(7) no N1 C2 C12 C11 . . . . -150.8(7) no N1 C2 C12 C25 . . . . 91.5(8) no N1 C6 C5 C4 . . . . 13.1(10) no N1 C6 C5 C7 . . . . 136.7(7) no N1 C6 C9 C8 . . . . -138.4(7) no N1 C6 C21 C22 . . . . -57.2(10) no N1 C6 C21 C23 . . . . -177.2(9) no N1 C6 C21 C24 . . . . 59.5(10) no C2 N1 C6 C5 . . . . -55.6(9) no C2 N1 C6 C9 . . . . 61.5(9) no C2 N1 C6 C21 . . . . -178.3(7) no C2 C3 C4 C5 . . . . -65.2(8) no C2 C3 C10 C11 . . . . -15.7(9) no C2 C3 C10 C13 . . . . 161.3(7) no C2 C12 C11 C10 . . . . 18.0(9) no C2 C12 C25 C26 . . . . -121.5(9) no C3 C2 N1 C6 . . . . 35.0(9) no C3 C2 C12 C11 . . . . -26.2(8) no C3 C2 C12 C25 . . . . -143.9(7) no C3 C4 C5 C6 . . . . 45.1(9) no C3 C4 C5 C7 . . . . -73.0(8) no C3 C10 C11 C12 . . . . -1.6(10) no C3 C10 C13 C14 . . . . 76.6(11) no C3 C10 C13 C15 . . . . -46.7(11) no C3 C10 C13 C16 . . . . -164.8(9) no C4 C3 C2 C12 . . . . -98.5(7) no C4 C3 C10 C11 . . . . 104.0(8) no C4 C3 C10 C13 . . . . -79.0(10) no C4 C5 C6 C9 . . . . -108.2(8) no C4 C5 C6 C21 . . . . 133.9(7) no C4 C5 C7 C8 . . . . 111.5(9) no C4 C5 C7 C17 . . . . -71.6(10) no C5 C4 C3 C10 . . . . 178.7(7) no C5 C6 C9 C8 . . . . -15.4(8) no C5 C6 C21 C22 . . . . 178.1(8) no C5 C6 C21 C23 . . . . 58.1(10) no C5 C6 C21 C24 . . . . -65.2(9) no C5 C7 C8 C9 . . . . -0.6(11) no C5 C7 C17 C18 . . . . -36.1(12) no C5 C7 C17 C19 . . . . -155.8(9) no C5 C7 C17 C20 . . . . 84.5(12) no C6 N1 C2 C12 . . . . 154.3(7) no C6 C5 C7 C8 . . . . -9.7(10) no C6 C5 C7 C17 . . . . 167.2(7) no C6 C9 C8 C7 . . . . 10.8(11) no C7 C5 C6 C9 . . . . 15.4(8) no C7 C5 C6 C21 . . . . -102.5(7) no C8 C7 C17 C18 . . . . 140.4(10) no C8 C7 C17 C19 . . . . 20.7(13) no C8 C7 C17 C20 . . . . -99.0(12) no C8 C9 C6 C21 . . . . 103.1(8) no C9 C6 C21 C22 . . . . 63.8(10) no C9 C6 C21 C23 . . . . -56.2(11) no C9 C6 C21 C24 . . . . -179.5(8) no C9 C8 C7 C17 . . . . -177.4(8) no C10 C3 C2 C12 . . . . 26.2(8) no C10 C11 C12 C25 . . . . 137.7(8) no C11 C10 C13 C14 . . . . -106.9(11) no C11 C10 C13 C15 . . . . 129.8(11) no C11 C10 C13 C16 . . . . 11.7(14) no C11 C12 C25 C26 . . . . 126.9(9) no C12 C11 C10 C13 . . . . -178.4(8) no C12 C25 C26 C27 . . . . 57.4(12) no C12 C25 C26 C28 . . . . 178.0(9) no C12 C25 C26 C29 . . . . -63.4(11) no #============================================================================== # End of CIF #==============================================================================