Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' loop_ _publ_author_name 'Ooyama, Yousuke' 'Tanikawa, Sachiko' 'Watanabe, Shigeru' 'Yoshida, Katsuhira' _publ_contact_author_name 'Prof Katsuhira Yoshida' _publ_contact_author_address ; Department of Material Science Kochi University Akebono-cho Kochi 780 8520 JAPAN ; _publ_contact_author_email 'KYOSHIDA@CC.KOCHI-U.AC.JP' #------------------------------------------------------------------------------ _publ_requested_journal 'Journal of the Chemical Society; Perkin Transactions 2' _publ_section_title ; Heterocyclicquinol-type fluorophores. Part 2. Solid-state fluorescence enhancement behaviour of benzofurano[3, 2-b]naphthoquinol-type clathrate hosts upon inclusion of amine molecules ; data_ 2c·morpholine _database_code_CSD 172464 #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_formula_sum 'C34 H40 N2 O4 ' _chemical_formula_weight 540.70 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _cell_length_a 25.87(1) _cell_length_b 11.844(2) _cell_length_c 20.729(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.94(2) _cell_angle_gamma 90.00 _cell_volume 6006(3) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.196 _diffrn_radiation_type 'Mo K„a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 4 _cell_measurement_theta_min 11.1 _cell_measurement_theta_max 11.2 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_F_000 2320.00 _exptl_absorpt_coefficient_mu 0.078 _exptl_crystal_description 'prismatic' _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_colour 'yellow' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method „w-2„q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.921 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_radiation_monochromator graphite _diffrn_reflns_number 3470 _reflns_number_total 3385 _diffrn_reflns_theta_max 22.5 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.505 _refine_ls_number_reflns 1119 _refine_ls_number_parameters 429 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[„s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0125 _refine_ls_shift/su_mean 0.0011 _refine_diff_density_min -0.14 _refine_diff_density_max 0.17 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.6041(5) 0.208(1) 0.1917(5) 0.090(5) Uani 1.00 d . . . O(2) O 0.4770(3) 0.1060(7) -0.0600(4) 0.092(3) Uani 1.00 d . . . O(3) O 0.5930(3) 0.1020(6) -0.0223(3) 0.060(3) Uani 1.00 d . . . O(4) O 0.6558(7) -0.122(1) 0.3050(7) 0.187(7) Uani 1.00 d . . . N(1) N 0.7865(5) 0.079(1) 0.0181(6) 0.113(5) Uani 1.00 d . . . N(2) N 0.5911(7) -0.0179(10) 0.1850(7) 0.117(6) Uani 1.00 d . . . C(1) C 0.5763(4) 0.252(1) 0.1254(5) 0.057(5) Uani 1.00 d . . . C(2) C 0.5159(5) 0.233(1) 0.1112(7) 0.062(5) Uani 1.00 d . . . C(3) C 0.4896(6) 0.266(1) 0.1568(6) 0.080(6) Uani 1.00 d . . . C(4) C 0.4352(7) 0.250(1) 0.1447(8) 0.092(6) Uani 1.00 d . . . C(5) C 0.4034(5) 0.206(1) 0.0842(9) 0.080(5) Uani 1.00 d . . . C(6) C 0.4266(6) 0.1719(10) 0.0367(6) 0.070(5) Uani 1.00 d . . . C(7) C 0.4824(6) 0.1849(10) 0.0491(7) 0.057(5) Uani 1.00 d . . . C(8) C 0.5058(5) 0.1422(9) -0.0032(7) 0.062(5) Uani 1.00 d . . . C(9) C 0.5640(5) 0.1476(8) 0.0175(6) 0.052(4) Uani 1.00 d . . . C(10) C 0.6473(5) 0.1162(9) 0.0143(6) 0.054(4) Uani 1.00 d . . . C(11) C 0.6908(7) 0.083(1) -0.0049(6) 0.068(5) Uani 1.00 d . . . C(12) C 0.7426(6) 0.104(1) 0.0391(8) 0.081(5) Uani 1.00 d . . . C(13) C 0.7485(5) 0.161(1) 0.0996(8) 0.095(6) Uani 1.00 d . . . C(14) C 0.7052(6) 0.191(1) 0.1186(6) 0.078(5) Uani 1.00 d . . . C(15) C 0.6524(5) 0.1707(9) 0.0756(6) 0.054(4) Uani 1.00 d . . . C(16) C 0.5981(5) 0.1918(8) 0.0762(5) 0.051(4) Uani 1.00 d . . . C(17) C 0.5872(5) 0.379(1) 0.1228(7) 0.055(5) Uani 1.00 d . . . C(18) C 0.5661(5) 0.433(1) 0.0606(7) 0.070(6) Uani 1.00 d . . . C(19) C 0.5734(5) 0.545(1) 0.0545(7) 0.081(5) Uani 1.00 d . . . C(20) C 0.6012(7) 0.609(1) 0.111(1) 0.103(7) Uani 1.00 d . . . C(21) C 0.6228(7) 0.556(2) 0.1730(10) 0.108(8) Uani 1.00 d . . . C(22) C 0.6150(5) 0.441(1) 0.1799(7) 0.084(6) Uani 1.00 d . . . C(23) C 0.7818(6) 0.023(2) -0.0451(8) 0.099(7) Uani 1.00 d . . . C(24) C 0.7717(6) -0.104(2) -0.0477(7) 0.108(7) Uani 1.00 d . . . C(25) C 0.7529(6) -0.153(2) -0.1189(9) 0.112(7) Uani 1.00 d . . . C(26) C 0.7472(6) -0.281(1) -0.1230(8) 0.144(8) Uani 1.00 d . . . C(27) C 0.8492(9) 0.124(1) 0.0629(10) 0.145(9) Uani 1.00 d . . . C(28) C 0.862(1) 0.034(2) 0.101(1) 0.17(1) Uani 1.00 d . . . C(29) C 0.9270(8) 0.086(2) 0.1615(10) 0.176(9) Uani 1.00 d . . . C(30) C 0.9666(8) 0.124(2) 0.1404(9) 0.24(1) Uani 1.00 d . . . C(31) C 0.610(1) -0.060(2) 0.303(1) 0.18(1) Uani 1.00 d . . . C(32) C 0.5718(7) -0.057(2) 0.238(1) 0.177(9) Uani 1.00 d . . . C(33) C 0.641(1) -0.079(2) 0.1914(9) 0.167(9) Uani 1.00 d . . . C(34) C 0.6785(8) -0.083(2) 0.255(1) 0.21(1) Uani 1.00 d . . . H(1) H 0.613(3) 0.235(7) 0.209(4) -0.04(1) Uiso 1.00 calc . . . H(2) H 0.606(6) 0.04(1) 0.197(7) 0.1091 Uiso 1.00 calc . . . H(3) H 0.511(3) 0.295(7) 0.197(3) 0.03(1) Uiso 1.00 calc . . . H(4) H 0.4193 0.2741 0.1779 0.1166 Uiso 1.00 calc . . . H(5) H 0.365(4) 0.198(8) 0.075(5) 0.090(9) Uiso 1.00 calc . . . H(6) H 0.404(3) 0.129(7) -0.005(4) 0.062(10) Uiso 1.00 calc . . . H(7) H 0.685(4) 0.051(8) -0.040(4) 0.052(8) Uiso 1.00 calc . . . H(8) H 0.782(3) 0.161(7) 0.128(4) 0.03(1) Uiso 1.00 calc . . . H(9) H 0.711(2) 0.224(5) 0.156(3) -0.01(1) Uiso 1.00 calc . . . H(10) H 0.549(4) 0.388(8) 0.024(4) 0.068(8) Uiso 1.00 calc . . . H(11) H 0.5601 0.5811 0.0085 0.1047 Uiso 1.00 calc . . . H(12) H 0.6062 0.6884 0.1065 0.1316 Uiso 1.00 calc . . . H(13) H 0.638(4) 0.604(9) 0.207(5) 0.107(7) Uiso 1.00 calc . . . H(14) H 0.637(4) 0.398(9) 0.221(5) 0.092(7) Uiso 1.00 calc . . . H(15) H 0.818(4) 0.055(8) -0.049(5) 0.098(8) Uiso 1.00 calc . . . H(16) H 0.754(3) 0.054(7) -0.081(4) 0.03(1) Uiso 1.00 calc . . . H(17) H 0.8057 -0.1416 -0.0209 0.1294 Uiso 1.00 calc . . . H(18) H 0.7455 -0.1192 -0.0255 0.1294 Uiso 1.00 calc . . . H(19) H 0.713(4) -0.128(10) -0.137(5) 0.118(7) Uiso 1.00 calc . . . H(20) H 0.777(6) -0.15(2) -0.135(8) 0.206(3) Uiso 1.00 calc . . . H(21) H 0.7819 -0.3166 -0.1004 0.1827 Uiso 1.00 calc . . . H(22) H 0.7344 -0.3050 -0.1687 0.1827 Uiso 1.00 calc . . . H(23) H 0.7222 -0.3056 -0.1002 0.1827 Uiso 1.00 calc . . . H(24) H 0.8484 0.1901 0.0882 0.1727 Uiso 1.00 calc . . . H(25) H 0.8720 0.1360 0.0356 0.1727 Uiso 1.00 calc . . . H(26) H 0.846(3) 0.031(7) 0.129(3) 0.02(1) Uiso 1.00 calc . . . H(27) H 0.877(4) -0.040(9) 0.081(5) 0.105(8) Uiso 1.00 calc . . . H(28) H 0.9403 0.0255 0.1924 0.2202 Uiso 1.00 calc . . . H(29) H 0.9164 0.1468 0.1839 0.2202 Uiso 1.00 calc . . . H(30) H 0.9553 0.1855 0.1128 0.2922 Uiso 1.00 calc . . . H(31) H 0.9971 0.1383 0.1792 0.2922 Uiso 1.00 calc . . . H(32) H 0.9763 0.0624 0.1149 0.2922 Uiso 1.00 calc . . . H(33) H 0.5929 -0.0864 0.3357 0.2185 Uiso 1.00 calc . . . H(34) H 0.6189 0.0211 0.3164 0.2185 Uiso 1.00 calc . . . H(35) H 0.5571 -0.1325 0.2269 0.2033 Uiso 1.00 calc . . . H(36) H 0.5390 -0.0109 0.2373 0.2033 Uiso 1.00 calc . . . H(37) H 0.6560 -0.0536 0.1550 0.1925 Uiso 1.00 calc . . . H(38) H 0.6299 -0.1591 0.1764 0.1925 Uiso 1.00 calc . . . H(39) H 0.6926 -0.0038 0.2627 0.2482 Uiso 1.00 calc . . . H(40) H 0.7102 -0.1262 0.2532 0.2482 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) 0.079(8) 0.12(1) 0.058(9) 0.003(7) 0.008(7) -0.017(7) O(2) 0.069(6) 0.112(7) 0.082(6) -0.005(6) 0.006(5) -0.016(6) O(3) 0.056(6) 0.061(5) 0.054(5) 0.003(5) 0.006(4) -0.006(4) O(4) 0.22(2) 0.22(1) 0.098(10) 0.09(1) 0.02(1) 0.038(9) N(1) 0.071(9) 0.18(1) 0.089(9) -0.001(9) 0.030(8) -0.050(9) N(2) 0.15(1) 0.09(1) 0.09(1) 0.00(1) 0.000(9) 0.030(9) C(1) 0.046(9) 0.08(1) 0.033(8) -0.001(8) -0.005(6) 0.003(8) C(2) 0.058(10) 0.067(9) 0.059(8) -0.006(8) 0.015(9) 0.011(8) C(3) 0.08(1) 0.09(1) 0.077(10) -0.004(10) 0.041(10) -0.011(9) C(4) 0.06(1) 0.11(1) 0.11(1) 0.005(9) 0.038(9) 0.03(1) C(5) 0.043(9) 0.09(1) 0.10(1) 0.006(10) 0.02(1) 0.026(10) C(6) 0.07(1) 0.056(9) 0.09(1) 0.005(8) 0.034(9) -0.003(8) C(7) 0.054(10) 0.038(8) 0.09(1) 0.016(7) 0.043(10) 0.018(7) C(8) 0.037(10) 0.044(9) 0.09(1) 0.006(8) 0.009(8) 0.020(8) C(9) 0.067(10) 0.045(8) 0.050(8) 0.004(7) 0.028(8) -0.013(6) C(10) 0.038(8) 0.059(8) 0.056(9) 0.000(7) 0.002(7) -0.017(7) C(11) 0.069(10) 0.08(1) 0.053(9) 0.006(9) 0.02(1) -0.013(8) C(12) 0.06(1) 0.11(1) 0.072(10) 0.001(9) 0.017(10) -0.005(10) C(13) 0.05(1) 0.16(1) 0.07(1) 0.00(1) 0.016(9) -0.04(1) C(14) 0.09(1) 0.10(1) 0.045(9) -0.010(10) 0.02(1) -0.043(8) C(15) 0.051(9) 0.053(9) 0.054(8) -0.008(7) 0.012(7) -0.007(7) C(16) 0.059(10) 0.049(8) 0.045(8) -0.011(7) 0.016(7) -0.005(7) C(17) 0.054(8) 0.044(9) 0.081(10) -0.008(7) 0.039(7) -0.015(9) C(18) 0.08(1) 0.05(1) 0.09(1) 0.006(8) 0.034(9) 0.004(9) C(19) 0.09(1) 0.07(1) 0.08(1) 0.001(8) 0.026(8) -0.012(9) C(20) 0.13(1) 0.08(1) 0.13(1) 0.00(1) 0.08(1) -0.01(1) C(21) 0.14(2) 0.08(2) 0.14(2) -0.05(1) 0.08(1) -0.06(1) C(22) 0.08(1) 0.10(1) 0.08(1) -0.02(1) 0.024(8) -0.02(1) C(23) 0.07(1) 0.13(2) 0.10(1) 0.00(1) 0.032(10) -0.01(1) C(24) 0.11(1) 0.15(2) 0.08(1) 0.03(1) 0.056(9) 0.01(1) C(25) 0.11(1) 0.14(2) 0.10(1) 0.02(1) 0.05(1) -0.01(1) C(26) 0.18(2) 0.12(1) 0.17(2) 0.00(1) 0.09(1) -0.03(1) C(27) 0.25(2) 0.08(1) 0.15(2) 0.03(1) 0.13(2) 0.03(1) C(28) 0.25(3) 0.10(2) 0.23(3) 0.06(2) 0.19(2) 0.04(2) C(29) 0.11(2) 0.18(2) 0.20(2) 0.01(2) 0.00(1) -0.01(2) C(30) 0.13(2) 0.46(4) 0.16(2) 0.06(2) 0.09(1) 0.12(2) C(31) 0.22(2) 0.27(3) 0.09(1) 0.03(2) 0.07(2) 0.01(2) C(32) 0.15(2) 0.23(2) 0.12(2) -0.04(2) 0.00(1) 0.06(2) C(33) 0.23(2) 0.14(2) 0.10(1) 0.06(2) 0.01(2) 0.00(1) C(34) 0.15(2) 0.36(3) 0.11(2) 0.09(2) 0.03(2) -0.01(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) 1.43(1) 1_555 1_555 yes O(2) C(8) 1.25(1) 1_555 1_555 yes O(3) C(9) 1.390(10) 1_555 1_555 yes O(3) C(10) 1.37(1) 1_555 1_555 yes O(4) C(31) 1.40(2) 1_555 1_555 yes O(4) C(34) 1.42(2) 1_555 1_555 yes N(1) C(12) 1.38(1) 1_555 1_555 yes N(1) C(23) 1.44(2) 1_555 1_555 yes N(1) C(27) 1.67(2) 1_555 1_555 yes N(2) C(32) 1.43(2) 1_555 1_555 yes N(2) C(33) 1.45(2) 1_555 1_555 yes C(1) C(2) 1.51(1) 1_555 1_555 yes C(1) C(16) 1.50(1) 1_555 1_555 yes C(1) C(17) 1.54(1) 1_555 1_555 yes C(2) C(3) 1.39(1) 1_555 1_555 yes C(2) C(7) 1.42(1) 1_555 1_555 yes C(3) C(4) 1.36(1) 1_555 1_555 yes C(4) C(5) 1.36(2) 1_555 1_555 yes C(5) C(6) 1.37(1) 1_555 1_555 yes C(6) C(7) 1.39(1) 1_555 1_555 yes C(7) C(8) 1.49(1) 1_555 1_555 yes C(8) C(9) 1.43(1) 1_555 1_555 yes C(9) C(16) 1.35(1) 1_555 1_555 yes C(10) C(11) 1.37(1) 1_555 1_555 yes C(10) C(15) 1.39(1) 1_555 1_555 yes C(11) C(12) 1.38(1) 1_555 1_555 yes C(12) C(13) 1.39(1) 1_555 1_555 yes C(13) C(14) 1.35(1) 1_555 1_555 yes C(14) C(15) 1.39(1) 1_555 1_555 yes C(15) C(16) 1.43(1) 1_555 1_555 yes C(17) C(18) 1.38(1) 1_555 1_555 yes C(17) C(22) 1.38(1) 1_555 1_555 yes C(18) C(19) 1.35(2) 1_555 1_555 yes C(19) C(20) 1.38(2) 1_555 1_555 yes C(20) C(21) 1.38(2) 1_555 1_555 yes C(21) C(22) 1.39(2) 1_555 1_555 yes C(23) C(24) 1.52(2) 1_555 1_555 yes C(24) C(25) 1.51(2) 1_555 1_555 yes C(25) C(26) 1.53(2) 1_555 1_555 yes C(27) C(28) 1.31(2) 1_555 1_555 yes C(28) C(29) 1.84(3) 1_555 1_555 yes C(29) C(30) 1.32(2) 1_555 1_555 yes C(31) C(32) 1.38(2) 1_555 1_555 yes C(33) C(34) 1.36(2) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) O(1) H(1) 116(11) 1_555 1_555 1_555 no C(9) O(3) C(10) 106.0(9) 1_555 1_555 1_555 yes C(31) O(4) C(34) 111(1) 1_555 1_555 1_555 yes C(12) N(1) C(23) 123(1) 1_555 1_555 1_555 yes C(12) N(1) C(27) 120(1) 1_555 1_555 1_555 yes C(23) N(1) C(27) 115(1) 1_555 1_555 1_555 yes C(32) N(2) C(33) 107(1) 1_555 1_555 1_555 yes C(32) N(2) H(2) 106(10) 1_555 1_555 1_555 no C(33) N(2) H(2) 95(11) 1_555 1_555 1_555 no O(1) C(1) C(2) 107.4(10) 1_555 1_555 1_555 yes O(1) C(1) C(16) 107(1) 1_555 1_555 1_555 yes O(1) C(1) C(17) 110(1) 1_555 1_555 1_555 yes C(2) C(1) C(16) 112(1) 1_555 1_555 1_555 yes C(2) C(1) C(17) 109.4(10) 1_555 1_555 1_555 yes C(16) C(1) C(17) 109.2(9) 1_555 1_555 1_555 yes C(1) C(2) C(3) 121(1) 1_555 1_555 1_555 yes C(1) C(2) C(7) 121(1) 1_555 1_555 1_555 yes C(3) C(2) C(7) 116(1) 1_555 1_555 1_555 yes C(2) C(3) C(4) 122(1) 1_555 1_555 1_555 yes C(2) C(3) H(3) 116(5) 1_555 1_555 1_555 no C(4) C(3) H(3) 120(5) 1_555 1_555 1_555 no C(3) C(4) C(5) 120(1) 1_555 1_555 1_555 yes C(3) C(4) H(4) 119(1) 1_555 1_555 1_555 no C(5) C(4) H(4) 120(1) 1_555 1_555 1_555 no C(4) C(5) C(6) 120(1) 1_555 1_555 1_555 yes C(4) C(5) H(5) 120(6) 1_555 1_555 1_555 no C(6) C(5) H(5) 119(5) 1_555 1_555 1_555 no C(5) C(6) C(7) 120(1) 1_555 1_555 1_555 yes C(5) C(6) H(6) 120(5) 1_555 1_555 1_555 no C(7) C(6) H(6) 119(5) 1_555 1_555 1_555 no C(2) C(7) C(6) 120(1) 1_555 1_555 1_555 yes C(2) C(7) C(8) 121(1) 1_555 1_555 1_555 yes C(6) C(7) C(8) 117(1) 1_555 1_555 1_555 yes O(2) C(8) C(7) 122(1) 1_555 1_555 1_555 yes O(2) C(8) C(9) 123(1) 1_555 1_555 1_555 yes C(7) C(8) C(9) 113(1) 1_555 1_555 1_555 yes O(3) C(9) C(8) 121(1) 1_555 1_555 1_555 yes O(3) C(9) C(16) 111(1) 1_555 1_555 1_555 yes C(8) C(9) C(16) 127(1) 1_555 1_555 1_555 yes O(3) C(10) C(11) 126(1) 1_555 1_555 1_555 yes O(3) C(10) C(15) 109(1) 1_555 1_555 1_555 yes C(11) C(10) C(15) 123(1) 1_555 1_555 1_555 yes C(10) C(11) C(12) 117(1) 1_555 1_555 1_555 yes C(10) C(11) H(7) 118(7) 1_555 1_555 1_555 no C(12) C(11) H(7) 123(7) 1_555 1_555 1_555 no N(1) C(12) C(11) 118(1) 1_555 1_555 1_555 yes N(1) C(12) C(13) 122(1) 1_555 1_555 1_555 yes C(11) C(12) C(13) 119(1) 1_555 1_555 1_555 yes C(12) C(13) C(14) 122(1) 1_555 1_555 1_555 yes C(12) C(13) H(8) 114(5) 1_555 1_555 1_555 no C(14) C(13) H(8) 122(5) 1_555 1_555 1_555 no C(13) C(14) C(15) 120(1) 1_555 1_555 1_555 yes C(13) C(14) H(9) 118(4) 1_555 1_555 1_555 no C(15) C(14) H(9) 120(4) 1_555 1_555 1_555 no C(10) C(15) C(14) 116(1) 1_555 1_555 1_555 yes C(10) C(15) C(16) 106(1) 1_555 1_555 1_555 yes C(14) C(15) C(16) 136(1) 1_555 1_555 1_555 yes C(1) C(16) C(9) 121(1) 1_555 1_555 1_555 yes C(1) C(16) C(15) 132(1) 1_555 1_555 1_555 yes C(9) C(16) C(15) 106.2(10) 1_555 1_555 1_555 yes C(1) C(17) C(18) 117(1) 1_555 1_555 1_555 yes C(1) C(17) C(22) 122(1) 1_555 1_555 1_555 yes C(18) C(17) C(22) 119(1) 1_555 1_555 1_555 yes C(17) C(18) C(19) 121(1) 1_555 1_555 1_555 yes C(17) C(18) H(10) 116(6) 1_555 1_555 1_555 no C(19) C(18) H(10) 122(6) 1_555 1_555 1_555 no C(18) C(19) C(20) 120(1) 1_555 1_555 1_555 yes C(18) C(19) H(11) 119(1) 1_555 1_555 1_555 no C(20) C(19) H(11) 120(1) 1_555 1_555 1_555 no C(19) C(20) C(21) 119(1) 1_555 1_555 1_555 yes C(19) C(20) H(12) 120(2) 1_555 1_555 1_555 no C(21) C(20) H(12) 120(2) 1_555 1_555 1_555 no C(20) C(21) C(22) 120(1) 1_555 1_555 1_555 yes C(20) C(21) H(13) 113(7) 1_555 1_555 1_555 no C(22) C(21) H(13) 125(8) 1_555 1_555 1_555 no C(17) C(22) C(21) 118(1) 1_555 1_555 1_555 yes C(17) C(22) H(14) 117(6) 1_555 1_555 1_555 no C(21) C(22) H(14) 121(6) 1_555 1_555 1_555 no N(1) C(23) C(24) 116(1) 1_555 1_555 1_555 yes N(1) C(23) H(15) 95(5) 1_555 1_555 1_555 no N(1) C(23) H(16) 111(5) 1_555 1_555 1_555 no C(24) C(23) H(15) 120(5) 1_555 1_555 1_555 no C(24) C(23) H(16) 105(5) 1_555 1_555 1_555 no H(15) C(23) H(16) 106(8) 1_555 1_555 1_555 no C(23) C(24) C(25) 114(1) 1_555 1_555 1_555 yes C(23) C(24) H(17) 108(1) 1_555 1_555 1_555 no C(23) C(24) H(18) 108(1) 1_555 1_555 1_555 no C(25) C(24) H(17) 108(1) 1_555 1_555 1_555 no C(25) C(24) H(18) 110(1) 1_555 1_555 1_555 no H(17) C(24) H(18) 106(1) 1_555 1_555 1_555 no C(24) C(25) C(26) 115(1) 1_555 1_555 1_555 yes C(24) C(25) H(19) 102(6) 1_555 1_555 1_555 no C(24) C(25) H(20) 108(12) 1_555 1_555 1_555 no C(26) C(25) H(19) 101(7) 1_555 1_555 1_555 no C(26) C(25) H(20) 98(13) 1_555 1_555 1_555 no H(19) C(25) H(20) 129(14) 1_555 1_555 1_555 no C(25) C(26) H(21) 110(1) 1_555 1_555 1_555 no C(25) C(26) H(22) 110(1) 1_555 1_555 1_555 no C(25) C(26) H(23) 109(1) 1_555 1_555 1_555 no H(21) C(26) H(22) 109(1) 1_555 1_555 1_555 no H(21) C(26) H(23) 107(1) 1_555 1_555 1_555 no H(22) C(26) H(23) 109(1) 1_555 1_555 1_555 no N(1) C(27) C(28) 95(1) 1_555 1_555 1_555 yes N(1) C(27) H(24) 112(1) 1_555 1_555 1_555 no N(1) C(27) H(25) 113(1) 1_555 1_555 1_555 no C(28) C(27) H(24) 112(1) 1_555 1_555 1_555 no C(28) C(27) H(25) 113(1) 1_555 1_555 1_555 no H(24) C(27) H(25) 109(1) 1_555 1_555 1_555 no C(27) C(28) C(29) 97(1) 1_555 1_555 1_555 yes C(27) C(28) H(26) 111(6) 1_555 1_555 1_555 no C(27) C(28) H(27) 117(5) 1_555 1_555 1_555 no C(29) C(28) H(26) 96(5) 1_555 1_555 1_555 no C(29) C(28) H(27) 100(5) 1_555 1_555 1_555 no H(26) C(28) H(27) 124(9) 1_555 1_555 1_555 no C(28) C(29) C(30) 121(1) 1_555 1_555 1_555 yes C(28) C(29) H(28) 104(1) 1_555 1_555 1_555 no C(28) C(29) H(29) 104(1) 1_555 1_555 1_555 no C(30) C(29) H(28) 109(1) 1_555 1_555 1_555 no C(30) C(29) H(29) 106(2) 1_555 1_555 1_555 no H(28) C(29) H(29) 110(2) 1_555 1_555 1_555 no C(29) C(30) H(30) 111(1) 1_555 1_555 1_555 no C(29) C(30) H(31) 107(1) 1_555 1_555 1_555 no C(29) C(30) H(32) 106(2) 1_555 1_555 1_555 no H(30) C(30) H(31) 113(2) 1_555 1_555 1_555 no H(30) C(30) H(32) 110(1) 1_555 1_555 1_555 no H(31) C(30) H(32) 107(1) 1_555 1_555 1_555 no O(4) C(31) C(32) 112(1) 1_555 1_555 1_555 yes O(4) C(31) H(33) 112(2) 1_555 1_555 1_555 no O(4) C(31) H(34) 111(2) 1_555 1_555 1_555 no C(32) C(31) H(33) 110(2) 1_555 1_555 1_555 no C(32) C(31) H(34) 105(2) 1_555 1_555 1_555 no H(33) C(31) H(34) 103(1) 1_555 1_555 1_555 no N(2) C(32) C(31) 116(1) 1_555 1_555 1_555 yes N(2) C(32) H(35) 108(2) 1_555 1_555 1_555 no N(2) C(32) H(36) 108(2) 1_555 1_555 1_555 no C(31) C(32) H(35) 108(1) 1_555 1_555 1_555 no C(31) C(32) H(36) 111(2) 1_555 1_555 1_555 no H(35) C(32) H(36) 103(1) 1_555 1_555 1_555 no N(2) C(33) C(34) 116(1) 1_555 1_555 1_555 yes N(2) C(33) H(37) 109(2) 1_555 1_555 1_555 no N(2) C(33) H(38) 106(2) 1_555 1_555 1_555 no C(34) C(33) H(37) 114(2) 1_555 1_555 1_555 no C(34) C(33) H(38) 107(1) 1_555 1_555 1_555 no H(37) C(33) H(38) 101(1) 1_555 1_555 1_555 no O(4) C(34) C(33) 112(1) 1_555 1_555 1_555 yes O(4) C(34) H(39) 113(1) 1_555 1_555 1_555 no O(4) C(34) H(40) 114(2) 1_555 1_555 1_555 no C(33) C(34) H(39) 103(2) 1_555 1_555 1_555 no C(33) C(34) H(40) 108(2) 1_555 1_555 1_555 no H(39) C(34) H(40) 103(2) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ #===============================================END data_ 2c·piperidine _database_code_CSD 172465 #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_formula_sum 'C35 H42 N2 O3 ' _chemical_formula_weight 538.73 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _cell_length_a 12.655(3) _cell_length_b 13.214(3) _cell_length_c 10.795(2) _cell_angle_alpha 100.55(2) _cell_angle_beta 101.92(2) _cell_angle_gamma 114.05(2) _cell_volume 1539.2(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.162 _diffrn_radiation_type 'Mo K„a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.7 _cell_measurement_theta_max 13.6 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_F_000 580.00 _exptl_absorpt_coefficient_mu 0.073 _exptl_crystal_description 'prismatic' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.250 _exptl_crystal_colour 'yellow' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method „w-2„q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.965 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_radiation_monochromator graphite _diffrn_reflns_number 4234 _reflns_number_total 4015 _diffrn_reflns_theta_max 22.51 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.317 _refine_ls_number_reflns 1967 _refine_ls_number_parameters 414 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[„s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 3.9864 _refine_ls_shift/su_mean 0.1290 _refine_diff_density_min -0.30 _refine_diff_density_max 0.38 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.1933(5) 0.4238(4) 0.1485(4) 0.070(2) Uani 1.00 d . . . O(2) O 0.4003(4) 0.4704(4) 0.6542(5) 0.084(2) Uani 1.00 d . . . O(3) O 0.4916(4) 0.6548(4) 0.5439(4) 0.072(2) Uani 1.00 d . . . N(1) N 0.6689(8) 0.9975(7) 0.4047(9) 0.118(3) Uani 1.00 d . . . N(2) N 0.6475(6) 0.6664(6) 0.8548(6) 0.073(2) Uani 1.00 d . . . C(1) C 0.1960(6) 0.4604(6) 0.2814(6) 0.062(2) Uani 1.00 d . . . C(2) C 0.1591(6) 0.3572(6) 0.3391(7) 0.054(2) Uani 1.00 d . . . C(3) C 0.0530(7) 0.2568(7) 0.2638(8) 0.073(3) Uani 1.00 d . . . C(4) C 0.0173(8) 0.1604(7) 0.313(1) 0.087(3) Uani 1.00 d . . . C(5) C 0.0821(7) 0.1642(7) 0.4323(9) 0.077(3) Uani 1.00 d . . . C(6) C 0.1862(7) 0.2621(7) 0.5044(8) 0.068(3) Uani 1.00 d . . . C(7) C 0.2281(6) 0.3616(6) 0.4606(6) 0.058(2) Uani 1.00 d . . . C(8) C 0.3433(6) 0.4649(6) 0.5437(7) 0.060(2) Uani 1.00 d . . . C(9) C 0.3805(6) 0.5529(6) 0.4826(7) 0.058(2) Uani 1.00 d . . . C(10) C 0.4966(7) 0.7208(7) 0.4563(7) 0.067(3) Uani 1.00 d . . . C(11) C 0.5914(7) 0.8303(6) 0.4828(9) 0.077(3) Uani 1.00 d . . . C(12) C 0.5801(8) 0.8857(7) 0.3878(10) 0.084(3) Uani 1.00 d . . . C(13) C 0.4810(9) 0.8286(8) 0.2730(10) 0.091(4) Uani 1.00 d . . . C(14) C 0.3886(8) 0.7198(8) 0.2500(8) 0.081(3) Uani 1.00 d . . . C(15) C 0.3938(6) 0.6625(6) 0.3458(7) 0.062(2) Uani 1.00 d . . . C(16) C 0.3214(6) 0.5554(6) 0.3635(6) 0.056(2) Uani 1.00 d . . . C(17) C 0.1015(6) 0.5061(6) 0.2817(7) 0.057(2) Uani 1.00 d . . . C(18) C 0.0978(7) 0.5656(6) 0.3979(8) 0.064(3) Uani 1.00 d . . . C(19) C 0.0116(8) 0.6021(7) 0.3995(9) 0.076(3) Uani 1.00 d . . . C(20) C -0.0756(8) 0.5802(9) 0.2850(10) 0.096(4) Uani 1.00 d . . . C(21) C -0.0704(8) 0.5226(9) 0.1674(9) 0.106(4) Uani 1.00 d . . . C(22) C 0.0163(8) 0.4843(8) 0.1656(8) 0.082(3) Uani 1.00 d . . . C(23) C 0.781(1) 1.0510(10) 0.519(2) 0.134(5) Uani 1.00 d . . . C(24) C 0.764(1) 1.103(1) 0.639(2) 0.131(6) Uani 1.00 d . . . C(25) C 0.864(1) 1.127(1) 0.763(2) 0.205(7) Uani 1.00 d . . . C(26) C 0.853(2) 1.161(2) 0.881(2) 0.28(1) Uani 1.00 d . . . C(27) C 0.657(2) 1.070(2) 0.323(2) 0.258(8) Uani 1.00 d . . . C(28) C 0.653(2) 1.115(2) 0.263(3) 0.38(1) Uani 1.00 d . . . C(29) C 0.631(5) 1.174(4) 0.170(7) 0.41(3) Uani 1.00 d . . . C(30) C 0.672(3) 1.252(4) 0.185(4) 0.41(2) Uani 1.00 d . . . C(31) C 0.5916(8) 0.6355(8) 0.9554(9) 0.100(3) Uani 1.00 d . . . C(32) C 0.6873(10) 0.6878(9) 1.0886(9) 0.115(4) Uani 1.00 d . . . C(33) C 0.762(1) 0.819(1) 1.122(1) 0.160(5) Uani 1.00 d . . . C(34) C 0.8102(10) 0.8485(8) 1.008(1) 0.125(4) Uani 1.00 d . . . C(35) C 0.7094(9) 0.7898(9) 0.8796(10) 0.106(4) Uani 1.00 d . . . H(1) H 0.261(5) 0.404(5) 0.145(5) 0.06(2) Uiso 1.00 calc . . . H(2) H 0.575(6) 0.636(5) 0.765(7) 0.09(2) Uiso 1.00 calc . . . H(3) H 0.005(5) 0.258(5) 0.179(6) 0.06(2) Uiso 1.00 calc . . . H(4) H -0.052(5) 0.086(5) 0.253(6) 0.06(2) Uiso 1.00 calc . . . H(5) H 0.0554 0.0993 0.4653 0.0929 Uiso 1.00 calc . . . H(6) H 0.233(5) 0.268(5) 0.582(6) 0.06(2) Uiso 1.00 calc . . . H(7) H 0.662(7) 0.866(6) 0.587(7) 0.11(2) Uiso 1.00 calc . . . H(8) H 0.457(7) 0.863(7) 0.188(8) 0.13(2) Uiso 1.00 calc . . . H(9) H 0.3214 0.6834 0.1697 0.0976 Uiso 1.00 calc . . . H(10) H 0.161(6) 0.592(5) 0.475(6) 0.07(2) Uiso 1.00 calc . . . H(11) H 0.004(5) 0.640(5) 0.480(6) 0.06(2) Uiso 1.00 calc . . . H(12) H -0.128(9) 0.626(8) 0.271(9) 0.17(2) Uiso 1.00 calc . . . H(13) H -0.1264 0.5106 0.0858 0.1297 Uiso 1.00 calc . . . H(14) H 0.023(6) 0.442(5) 0.094(6) 0.08(2) Uiso 1.00 calc . . . H(15) H 0.8049 0.9936 0.5327 0.1594 Uiso 1.00 calc . . . H(16) H 0.8439 1.1100 0.4989 0.1594 Uiso 1.00 calc . . . H(17) H 0.704(7) 1.069(7) 0.659(8) 0.10(2) Uiso 1.00 calc . . . H(18) H 0.757(8) 1.169(8) 0.613(8) 0.13(2) Uiso 1.00 calc . . . H(19) H 0.8738 1.0611 0.7566 0.2470 Uiso 1.00 calc . . . H(20) H 0.9357 1.1907 0.7615 0.2470 Uiso 1.00 calc . . . H(21) H 0.7864 1.0971 0.8907 0.3577 Uiso 1.00 calc . . . H(22) H 0.8419 1.2261 0.8925 0.3577 Uiso 1.00 calc . . . H(23) H 0.9263 1.1755 0.9474 0.3577 Uiso 1.00 calc . . . H(24) H 0.5653 1.0394 0.3141 0.2961 Uiso 1.00 calc . . . H(25) H 0.6894 1.1409 0.4064 0.2961 Uiso 1.00 calc . . . H(26) H 0.7287 1.1792 0.3188 0.4638 Uiso 1.00 calc . . . H(27) H 0.5863 1.1340 0.3176 0.3989 Uiso 1.00 calc . . . H(28) H 0.5566 1.1745 0.1840 0.6192 Uiso 1.00 calc . . . H(29) H 0.6223 1.1284 0.1000 0.6192 Uiso 1.00 calc . . . H(30) H 0.6264 1.2403 0.0856 0.4212 Uiso 1.00 calc . . . H(31) H 0.6643 1.2990 0.2369 0.4212 Uiso 1.00 calc . . . H(32) H 0.7492 1.2608 0.1786 0.4212 Uiso 1.00 calc . . . H(33) H 0.5514 0.5529 0.9358 0.1185 Uiso 1.00 calc . . . H(34) H 0.5332 0.6632 0.9570 0.1185 Uiso 1.00 calc . . . H(35) H 0.6504 0.6711 1.1548 0.1375 Uiso 1.00 calc . . . H(36) H 0.7420 0.6548 1.0878 0.1375 Uiso 1.00 calc . . . H(37) H 0.8273 0.8482 1.2009 0.1949 Uiso 1.00 calc . . . H(38) H 0.7102 0.8543 1.1332 0.1949 Uiso 1.00 calc . . . H(39) H 0.8707 0.8236 1.0040 0.1504 Uiso 1.00 calc . . . H(40) H 0.8469 0.9308 1.0231 0.1504 Uiso 1.00 calc . . . H(41) H 0.7413 0.8060 0.8093 0.1270 Uiso 1.00 calc . . . H(42) H 0.6521 0.8192 0.8826 0.1270 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) 0.078(4) 0.088(4) 0.047(3) 0.046(3) 0.015(3) 0.016(3) O(2) 0.083(4) 0.083(4) 0.064(3) 0.022(3) 0.007(3) 0.028(3) O(3) 0.063(3) 0.069(3) 0.070(3) 0.022(3) 0.013(3) 0.018(3) N(1) 0.106(6) 0.091(6) 0.154(8) 0.034(6) 0.036(6) 0.059(6) N(2) 0.064(4) 0.074(5) 0.070(4) 0.026(4) 0.011(4) 0.019(4) C(1) 0.066(5) 0.068(5) 0.044(4) 0.029(4) 0.012(4) 0.010(4) C(2) 0.056(4) 0.051(4) 0.061(4) 0.028(4) 0.020(4) 0.015(4) C(3) 0.059(5) 0.058(6) 0.080(6) 0.015(5) 0.011(5) 0.010(5) C(4) 0.054(5) 0.057(6) 0.121(8) 0.010(5) 0.028(6) -0.005(6) C(5) 0.064(5) 0.065(6) 0.100(7) 0.026(5) 0.022(5) 0.028(5) C(6) 0.067(6) 0.076(6) 0.065(6) 0.036(5) 0.020(5) 0.022(5) C(7) 0.069(5) 0.055(5) 0.054(4) 0.029(4) 0.020(4) 0.021(4) C(8) 0.060(5) 0.060(5) 0.059(5) 0.026(4) 0.014(4) 0.025(4) C(9) 0.042(4) 0.051(4) 0.061(5) 0.011(4) 0.008(4) 0.008(4) C(10) 0.071(5) 0.071(5) 0.077(5) 0.037(5) 0.035(5) 0.041(5) C(11) 0.072(6) 0.054(5) 0.106(7) 0.023(5) 0.034(5) 0.033(5) C(12) 0.073(6) 0.057(6) 0.123(8) 0.022(5) 0.037(6) 0.038(6) C(13) 0.097(7) 0.088(7) 0.100(7) 0.043(6) 0.040(6) 0.046(6) C(14) 0.090(6) 0.086(6) 0.079(5) 0.045(5) 0.028(5) 0.038(5) C(15) 0.063(5) 0.066(5) 0.059(5) 0.031(4) 0.015(4) 0.026(4) C(16) 0.049(4) 0.062(5) 0.050(4) 0.020(4) 0.012(4) 0.014(4) C(17) 0.058(4) 0.059(4) 0.059(4) 0.030(4) 0.016(4) 0.023(4) C(18) 0.070(5) 0.067(5) 0.060(5) 0.035(5) 0.021(4) 0.016(4) C(19) 0.094(6) 0.077(6) 0.073(6) 0.047(5) 0.036(5) 0.025(5) C(20) 0.104(7) 0.126(8) 0.089(7) 0.073(6) 0.033(6) 0.046(6) C(21) 0.100(7) 0.162(9) 0.076(6) 0.084(7) 0.016(5) 0.037(6) C(22) 0.084(6) 0.113(7) 0.062(6) 0.064(6) 0.015(5) 0.013(5) C(23) 0.102(9) 0.100(8) 0.23(1) 0.039(7) 0.087(10) 0.082(9) C(24) 0.14(1) 0.082(9) 0.19(1) 0.045(9) 0.09(1) 0.054(9) C(25) 0.13(1) 0.22(2) 0.19(2) 0.05(1) -0.04(1) 0.06(1) C(26) 0.29(2) 0.36(3) 0.11(1) 0.16(2) -0.06(1) -0.01(2) C(27) 0.27(2) 0.14(1) 0.20(2) -0.03(1) -0.04(1) 0.12(1) C(28) 0.32(3) 0.25(2) 0.39(4) 0.02(2) -0.12(2) 0.21(2) C(29) 0.50(5) 0.32(5) 0.55(7) 0.25(4) 0.15(5) 0.33(6) C(30) 0.30(4) 0.37(5) 0.68(5) 0.28(4) 0.08(3) 0.21(4) C(31) 0.081(6) 0.116(7) 0.076(6) 0.027(5) 0.022(5) 0.018(5) C(32) 0.138(9) 0.123(9) 0.072(6) 0.049(7) 0.034(6) 0.023(6) C(33) 0.18(1) 0.13(1) 0.121(10) 0.061(9) 0.033(9) -0.029(8) C(34) 0.137(9) 0.084(7) 0.116(9) 0.029(7) 0.023(8) 0.011(6) C(35) 0.125(8) 0.111(8) 0.104(7) 0.068(7) 0.035(6) 0.041(6) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(1) 1.418(7) 1_555 1_555 yes O(2) C(8) 1.232(7) 1_555 1_555 yes O(3) C(9) 1.406(7) 1_555 1_555 yes O(3) C(10) 1.393(7) 1_555 1_555 yes N(1) C(12) 1.393(10) 1_555 1_555 yes N(1) C(23) 1.47(1) 1_555 1_555 yes N(1) C(27) 1.45(2) 1_555 1_555 yes N(2) C(31) 1.446(9) 1_555 1_555 yes N(2) C(35) 1.43(1) 1_555 1_555 yes C(1) C(2) 1.541(9) 1_555 1_555 yes C(1) C(16) 1.506(9) 1_555 1_555 yes C(1) C(17) 1.544(9) 1_555 1_555 yes C(2) C(3) 1.388(9) 1_555 1_555 yes C(2) C(7) 1.394(8) 1_555 1_555 yes C(3) C(4) 1.41(1) 1_555 1_555 yes C(4) C(5) 1.36(1) 1_555 1_555 yes C(5) C(6) 1.355(10) 1_555 1_555 yes C(6) C(7) 1.413(9) 1_555 1_555 yes C(7) C(8) 1.477(9) 1_555 1_555 yes C(8) C(9) 1.403(9) 1_555 1_555 yes C(9) C(16) 1.362(8) 1_555 1_555 yes C(10) C(11) 1.382(9) 1_555 1_555 yes C(10) C(15) 1.383(9) 1_555 1_555 yes C(11) C(12) 1.38(1) 1_555 1_555 yes C(12) C(13) 1.39(1) 1_555 1_555 yes C(13) C(14) 1.37(1) 1_555 1_555 yes C(14) C(15) 1.395(9) 1_555 1_555 yes C(15) C(16) 1.411(9) 1_555 1_555 yes C(17) C(18) 1.374(9) 1_555 1_555 yes C(17) C(22) 1.368(9) 1_555 1_555 yes C(18) C(19) 1.36(1) 1_555 1_555 yes C(19) C(20) 1.37(1) 1_555 1_555 yes C(20) C(21) 1.39(1) 1_555 1_555 yes C(21) C(22) 1.39(1) 1_555 1_555 yes C(23) C(24) 1.45(2) 1_555 1_555 yes C(24) C(25) 1.51(2) 1_555 1_555 yes C(25) C(26) 1.33(2) 1_555 1_555 yes C(27) C(28) 0.96(2) 1_555 1_555 yes C(28) C(29) 1.38(3) 1_555 1_555 yes C(29) C(30) 0.82(5) 1_555 1_555 yes C(31) C(32) 1.50(1) 1_555 1_555 yes C(32) C(33) 1.53(1) 1_555 1_555 yes C(33) C(34) 1.53(1) 1_555 1_555 yes C(34) C(35) 1.49(1) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) O(1) H(1) 110(3) 1_555 1_555 1_555 no C(9) O(3) C(10) 104.7(5) 1_555 1_555 1_555 yes C(12) N(1) C(23) 118.7(8) 1_555 1_555 1_555 yes C(12) N(1) C(27) 124(1) 1_555 1_555 1_555 yes C(23) N(1) C(27) 116.4(10) 1_555 1_555 1_555 yes C(31) N(2) C(35) 111.8(7) 1_555 1_555 1_555 yes C(31) N(2) H(2) 106(3) 1_555 1_555 1_555 no C(35) N(2) H(2) 104(3) 1_555 1_555 1_555 no O(1) C(1) C(2) 110.6(5) 1_555 1_555 1_555 yes O(1) C(1) C(16) 109.6(5) 1_555 1_555 1_555 yes O(1) C(1) C(17) 108.0(5) 1_555 1_555 1_555 yes C(2) C(1) C(16) 110.8(6) 1_555 1_555 1_555 yes C(2) C(1) C(17) 107.8(5) 1_555 1_555 1_555 yes C(16) C(1) C(17) 110.0(5) 1_555 1_555 1_555 yes C(1) C(2) C(3) 117.2(7) 1_555 1_555 1_555 yes C(1) C(2) C(7) 122.7(6) 1_555 1_555 1_555 yes C(3) C(2) C(7) 120.1(7) 1_555 1_555 1_555 yes C(2) C(3) C(4) 118.7(8) 1_555 1_555 1_555 yes C(2) C(3) H(3) 117(3) 1_555 1_555 1_555 no C(4) C(3) H(3) 124(3) 1_555 1_555 1_555 no C(3) C(4) C(5) 121.8(8) 1_555 1_555 1_555 yes C(3) C(4) H(4) 117(3) 1_555 1_555 1_555 no C(5) C(4) H(4) 120(3) 1_555 1_555 1_555 no C(4) C(5) C(6) 119.1(8) 1_555 1_555 1_555 yes C(4) C(5) H(5) 120.9(9) 1_555 1_555 1_555 no C(6) C(5) H(5) 120.0(9) 1_555 1_555 1_555 no C(5) C(6) C(7) 122.0(7) 1_555 1_555 1_555 yes C(5) C(6) H(6) 122(4) 1_555 1_555 1_555 no C(7) C(6) H(6) 115(3) 1_555 1_555 1_555 no C(2) C(7) C(6) 118.2(7) 1_555 1_555 1_555 yes C(2) C(7) C(8) 122.8(6) 1_555 1_555 1_555 yes C(6) C(7) C(8) 119.0(6) 1_555 1_555 1_555 yes O(2) C(8) C(7) 122.3(6) 1_555 1_555 1_555 yes O(2) C(8) C(9) 124.5(6) 1_555 1_555 1_555 yes C(7) C(8) C(9) 113.1(6) 1_555 1_555 1_555 yes O(3) C(9) C(8) 121.0(6) 1_555 1_555 1_555 yes O(3) C(9) C(16) 110.7(6) 1_555 1_555 1_555 yes C(8) C(9) C(16) 128.3(6) 1_555 1_555 1_555 yes O(3) C(10) C(11) 122.7(7) 1_555 1_555 1_555 yes O(3) C(10) C(15) 110.5(6) 1_555 1_555 1_555 yes C(11) C(10) C(15) 126.8(7) 1_555 1_555 1_555 yes C(10) C(11) C(12) 115.4(8) 1_555 1_555 1_555 yes C(10) C(11) H(7) 115(3) 1_555 1_555 1_555 no C(12) C(11) H(7) 128(3) 1_555 1_555 1_555 no N(1) C(12) C(11) 120.7(9) 1_555 1_555 1_555 yes N(1) C(12) C(13) 119.5(9) 1_555 1_555 1_555 yes C(11) C(12) C(13) 119.7(8) 1_555 1_555 1_555 yes C(12) C(13) C(14) 123.2(9) 1_555 1_555 1_555 yes C(12) C(13) H(8) 128(4) 1_555 1_555 1_555 no C(14) C(13) H(8) 108(4) 1_555 1_555 1_555 no C(13) C(14) C(15) 118.9(8) 1_555 1_555 1_555 yes C(13) C(14) H(9) 120.7(8) 1_555 1_555 1_555 no C(15) C(14) H(9) 120.4(8) 1_555 1_555 1_555 no C(10) C(15) C(14) 115.9(7) 1_555 1_555 1_555 yes C(10) C(15) C(16) 106.6(6) 1_555 1_555 1_555 yes C(14) C(15) C(16) 137.5(7) 1_555 1_555 1_555 yes C(1) C(16) C(9) 121.5(6) 1_555 1_555 1_555 yes C(1) C(16) C(15) 130.7(6) 1_555 1_555 1_555 yes C(9) C(16) C(15) 107.4(6) 1_555 1_555 1_555 yes C(1) C(17) C(18) 121.2(6) 1_555 1_555 1_555 yes C(1) C(17) C(22) 120.3(7) 1_555 1_555 1_555 yes C(18) C(17) C(22) 118.5(7) 1_555 1_555 1_555 yes C(17) C(18) C(19) 121.5(8) 1_555 1_555 1_555 yes C(17) C(18) H(10) 119(4) 1_555 1_555 1_555 no C(19) C(18) H(10) 118(4) 1_555 1_555 1_555 no C(18) C(19) C(20) 121.4(9) 1_555 1_555 1_555 yes C(18) C(19) H(11) 123(3) 1_555 1_555 1_555 no C(20) C(19) H(11) 114(3) 1_555 1_555 1_555 no C(19) C(20) C(21) 117.2(9) 1_555 1_555 1_555 yes C(19) C(20) H(12) 125(5) 1_555 1_555 1_555 no C(21) C(20) H(12) 113(5) 1_555 1_555 1_555 no C(20) C(21) C(22) 121.6(9) 1_555 1_555 1_555 yes C(20) C(21) H(13) 119.3(10) 1_555 1_555 1_555 no C(22) C(21) H(13) 119(1) 1_555 1_555 1_555 no C(17) C(22) C(21) 119.8(8) 1_555 1_555 1_555 yes C(17) C(22) H(14) 113(4) 1_555 1_555 1_555 no C(21) C(22) H(14) 127(4) 1_555 1_555 1_555 no N(1) C(23) C(24) 111(1) 1_555 1_555 1_555 yes N(1) C(23) H(15) 109(1) 1_555 1_555 1_555 no N(1) C(23) H(16) 108(1) 1_555 1_555 1_555 no C(24) C(23) H(15) 109(1) 1_555 1_555 1_555 no C(24) C(23) H(16) 108(1) 1_555 1_555 1_555 no H(15) C(23) H(16) 109(1) 1_555 1_555 1_555 no C(23) C(24) C(25) 112(1) 1_555 1_555 1_555 yes C(23) C(24) H(17) 119(6) 1_555 1_555 1_555 no C(23) C(24) H(18) 98(5) 1_555 1_555 1_555 no C(25) C(24) H(17) 100(6) 1_555 1_555 1_555 no C(25) C(24) H(18) 119(5) 1_555 1_555 1_555 no H(17) C(24) H(18) 106(8) 1_555 1_555 1_555 no C(24) C(25) C(26) 119(1) 1_555 1_555 1_555 yes C(24) C(25) H(19) 107(1) 1_555 1_555 1_555 no C(24) C(25) H(20) 106(1) 1_555 1_555 1_555 no C(26) C(25) H(19) 108(1) 1_555 1_555 1_555 no C(26) C(25) H(20) 104(1) 1_555 1_555 1_555 no H(19) C(25) H(20) 110(1) 1_555 1_555 1_555 no C(25) C(26) H(21) 107(1) 1_555 1_555 1_555 no C(25) C(26) H(22) 112(2) 1_555 1_555 1_555 no C(25) C(26) H(23) 107(2) 1_555 1_555 1_555 no H(21) C(26) H(22) 111(2) 1_555 1_555 1_555 no H(21) C(26) H(23) 106(2) 1_555 1_555 1_555 no H(22) C(26) H(23) 110(1) 1_555 1_555 1_555 no N(1) C(27) C(28) 174(4) 1_555 1_555 1_555 yes N(1) C(27) H(24) 91(1) 1_555 1_555 1_555 no N(1) C(27) H(25) 91(1) 1_555 1_555 1_555 no C(28) C(27) H(24) 92(3) 1_555 1_555 1_555 no C(28) C(27) H(25) 92(3) 1_555 1_555 1_555 no H(24) C(27) H(25) 96(2) 1_555 1_555 1_555 no C(27) C(28) C(29) 171(5) 1_555 1_555 1_555 yes C(27) C(28) H(26) 91(2) 1_555 1_555 1_555 no C(27) C(28) H(27) 84(3) 1_555 1_555 1_555 no C(29) C(28) H(26) 91(2) 1_555 1_555 1_555 no C(29) C(28) H(27) 87(2) 1_555 1_555 1_555 no H(26) C(28) H(27) 98(2) 1_555 1_555 1_555 no C(28) C(29) C(30) 140(7) 1_555 1_555 1_555 yes C(28) C(29) H(28) 104(3) 1_555 1_555 1_555 no C(28) C(29) H(29) 96(2) 1_555 1_555 1_555 no C(30) C(29) H(28) 104(4) 1_555 1_555 1_555 no C(30) C(29) H(29) 100(8) 1_555 1_555 1_555 no H(28) C(29) H(29) 107(4) 1_555 1_555 1_555 no C(29) C(30) H(30) 108(7) 1_555 1_555 1_555 no C(29) C(30) H(31) 107(8) 1_555 1_555 1_555 no C(29) C(30) H(32) 110(4) 1_555 1_555 1_555 no H(30) C(30) H(31) 109(2) 1_555 1_555 1_555 no H(30) C(30) H(32) 109(5) 1_555 1_555 1_555 no H(31) C(30) H(32) 112(4) 1_555 1_555 1_555 no N(2) C(31) C(32) 109.8(7) 1_555 1_555 1_555 yes N(2) C(31) H(33) 109.6(8) 1_555 1_555 1_555 no N(2) C(31) H(34) 110.0(8) 1_555 1_555 1_555 no C(32) C(31) H(33) 109.3(9) 1_555 1_555 1_555 no C(32) C(31) H(34) 109.3(8) 1_555 1_555 1_555 no H(33) C(31) H(34) 108.8(8) 1_555 1_555 1_555 no C(31) C(32) C(33) 112.5(9) 1_555 1_555 1_555 yes C(31) C(32) H(35) 109.8(10) 1_555 1_555 1_555 no C(31) C(32) H(36) 108.5(8) 1_555 1_555 1_555 no C(33) C(32) H(35) 108(1) 1_555 1_555 1_555 no C(33) C(32) H(36) 107.6(10) 1_555 1_555 1_555 no H(35) C(32) H(36) 109.5(10) 1_555 1_555 1_555 no C(32) C(33) C(34) 109.6(8) 1_555 1_555 1_555 yes C(32) C(33) H(37) 110(1) 1_555 1_555 1_555 no C(32) C(33) H(38) 108(1) 1_555 1_555 1_555 no C(34) C(33) H(37) 110(1) 1_555 1_555 1_555 no C(34) C(33) H(38) 108(1) 1_555 1_555 1_555 no H(37) C(33) H(38) 109.7(10) 1_555 1_555 1_555 no C(33) C(34) C(35) 110.6(9) 1_555 1_555 1_555 yes C(33) C(34) H(39) 109(1) 1_555 1_555 1_555 no C(33) C(34) H(40) 109(1) 1_555 1_555 1_555 no C(35) C(34) H(39) 109.4(10) 1_555 1_555 1_555 no C(35) C(34) H(40) 109(1) 1_555 1_555 1_555 no H(39) C(34) H(40) 108(1) 1_555 1_555 1_555 no N(2) C(35) C(34) 111.7(8) 1_555 1_555 1_555 yes N(2) C(35) H(41) 108.9(9) 1_555 1_555 1_555 no N(2) C(35) H(42) 108.7(9) 1_555 1_555 1_555 no C(34) C(35) H(41) 109(1) 1_555 1_555 1_555 no C(34) C(35) H(42) 108.7(9) 1_555 1_555 1_555 no H(41) C(35) H(42) 109.4(9) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ #===============================================END data_ 3c·morpholine _database_code_CSD 172466 #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_formula_sum 'C34 H40 N2 O4 ' _chemical_formula_weight 540.70 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _cell_length_a 8.759(3) _cell_length_b 21.675(3) _cell_length_c 8.388(2) _cell_angle_alpha 99.77(1) _cell_angle_beta 109.72(2) _cell_angle_gamma 81.88(2) _cell_volume 1471.2(6) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.220 _diffrn_radiation_type 'Mo K„a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.3 _cell_measurement_theta_max 14.9 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_F_000 580.00 _exptl_absorpt_coefficient_mu 0.080 _exptl_crystal_description 'prismatic' _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.400 _exptl_crystal_colour 'yellow' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method „w-2„q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.968 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_radiation_monochromator graphite _diffrn_reflns_number 4138 _reflns_number_total 3833 _diffrn_reflns_theta_max 22.5 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 3.177 _refine_ls_number_reflns 2718 _refine_ls_number_parameters 418 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[„s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0038 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_min -0.62 _refine_diff_density_max 0.59 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O -0.4588(3) -0.3776(1) -0.6285(4) 0.0521(10) Uani 1.00 d . . . O(2) O -0.0250(4) -0.2057(2) -0.4130(5) 0.075(1) Uani 1.00 d . . . O(3) O -0.5176(3) -0.2600(1) -0.4246(4) 0.0468(9) Uani 1.00 d . . . O(4) O -0.8704(5) -0.3011(3) -1.0246(7) 0.120(2) Uani 1.00 d . . . N(1) N -0.7425(5) -0.0463(2) -0.2911(6) 0.063(1) Uani 1.00 d . . . N(2) N -0.5305(6) -0.3173(3) -0.9157(7) 0.090(2) Uani 1.00 d . . . C(1) C -0.3325(5) -0.3507(2) -0.4881(5) 0.043(1) Uani 1.00 d . . . C(2) C -0.1689(5) -0.3613(2) -0.5257(5) 0.045(1) Uani 1.00 d . . . C(3) C -0.1183(6) -0.4224(2) -0.5836(6) 0.052(2) Uani 1.00 d . . . C(4) C 0.0290(6) -0.4356(3) -0.6124(6) 0.060(2) Uani 1.00 d . . . C(5) C 0.1309(7) -0.3888(3) -0.5816(7) 0.065(2) Uani 1.00 d . . . C(6) C 0.0820(6) -0.3286(3) -0.5268(7) 0.060(2) Uani 1.00 d . . . C(7) C -0.0680(5) -0.3135(2) -0.4978(6) 0.049(1) Uani 1.00 d . . . C(8) C -0.1156(5) -0.2468(2) -0.4412(6) 0.051(1) Uani 1.00 d . . . C(9) C -0.2775(5) -0.2346(2) -0.4263(5) 0.047(1) Uani 1.00 d . . . C(10) C -0.3705(5) -0.1767(2) -0.3867(5) 0.046(1) Uani 1.00 d . . . C(11) C -0.3498(6) -0.1129(2) -0.3528(7) 0.057(2) Uani 1.00 d . . . C(12) C -0.4735(6) -0.0713(2) -0.3213(7) 0.059(2) Uani 1.00 d . . . C(13) C -0.6226(5) -0.0905(2) -0.3236(6) 0.050(1) Uani 1.00 d . . . C(14) C -0.6425(6) -0.1547(2) -0.3572(6) 0.048(1) Uani 1.00 d . . . C(15) C -0.5163(5) -0.1947(2) -0.3877(5) 0.045(1) Uani 1.00 d . . . C(16) C -0.3714(5) -0.2814(2) -0.4487(5) 0.044(1) Uani 1.00 d . . . C(17) C -0.3116(5) -0.3842(2) -0.3337(5) 0.044(1) Uani 1.00 d . . . C(18) C -0.2134(6) -0.3616(3) -0.1727(6) 0.060(2) Uani 1.00 d . . . C(19) C -0.1844(7) -0.3944(3) -0.0368(7) 0.074(2) Uani 1.00 d . . . C(20) C -0.2533(7) -0.4500(3) -0.0586(8) 0.071(2) Uani 1.00 d . . . C(21) C -0.3541(7) -0.4717(3) -0.2171(7) 0.066(2) Uani 1.00 d . . . C(22) C -0.3836(6) -0.4385(2) -0.3545(7) 0.057(2) Uani 1.00 d . . . C(23) C -0.7574(8) 0.0187(3) -0.3234(8) 0.080(2) Uani 1.00 d . . . C(24) C -0.7226(8) 0.0671(3) -0.1760(7) 0.078(2) Uani 1.00 d . . . C(25) C -0.7452(9) 0.1330(3) -0.2195(9) 0.099(3) Uani 1.00 d . . . C(26) C -0.751(1) 0.1842(3) -0.087(1) 0.123(3) Uani 1.00 d . . . C(27) C -0.8727(6) -0.0655(2) -0.2477(6) 0.060(2) Uani 1.00 d . . . C(28) C -0.819(1) -0.0847(5) -0.073(1) 0.167(4) Uani 1.00 d . . . C(29) C -0.832(2) -0.0689(7) 0.048(1) 0.313(8) Uani 1.00 d . . . C(30) C -0.787(1) -0.0857(4) 0.2240(9) 0.121(3) Uani 1.00 d . . . C(31) C -0.7881(9) -0.3589(4) -1.053(1) 0.119(3) Uani 1.00 d . . . C(32) C -0.6315(10) -0.3534(5) -1.0693(10) 0.140(4) Uani 1.00 d . . . C(33) C -0.6194(8) -0.2555(4) -0.889(1) 0.105(3) Uani 1.00 d . . . C(34) C -0.7744(8) -0.2657(3) -0.874(1) 0.112(3) Uani 1.00 d . . . H(1) H -0.471(7) -0.348(3) -0.724(8) 0.11(2) Uiso 1.00 calc . . . H(2) H -0.188(6) -0.453(2) -0.601(6) 0.06(1) Uiso 1.00 calc . . . H(3) H 0.067(6) -0.480(3) -0.655(6) 0.07(1) Uiso 1.00 calc . . . H(4) H 0.225(6) -0.398(2) -0.603(6) 0.07(2) Uiso 1.00 calc . . . H(5) H 0.143(6) -0.299(2) -0.504(6) 0.06(2) Uiso 1.00 calc . . . H(6) H -0.247(6) -0.099(2) -0.347(6) 0.08(2) Uiso 1.00 calc . . . H(7) H -0.464(6) -0.025(3) -0.314(7) 0.09(2) Uiso 1.00 calc . . . H(8) H -0.734(5) -0.169(2) -0.361(5) 0.05(1) Uiso 1.00 calc . . . H(9) H -0.158(6) -0.323(2) -0.154(6) 0.07(1) Uiso 1.00 calc . . . H(10) H -0.111(6) -0.381(2) 0.067(6) 0.07(2) Uiso 1.00 calc . . . H(11) H -0.240(6) -0.473(2) 0.030(6) 0.07(2) Uiso 1.00 calc . . . H(12) H -0.416(6) -0.509(3) -0.236(6) 0.08(2) Uiso 1.00 calc . . . H(13) H -0.444(6) -0.456(2) -0.476(6) 0.07(2) Uiso 1.00 calc . . . H(14) H -0.6936 0.0211 -0.3930 0.1020 Uiso 1.00 calc . . . H(15) H -0.8730 0.0276 -0.3954 0.1020 Uiso 1.00 calc . . . H(16) H -0.6212 0.0531 -0.0896 0.0380 Uiso 1.00 calc . . . H(17) H -0.7961 0.0604 -0.1152 0.0380 Uiso 1.00 calc . . . H(18) H -0.6737 0.1389 -0.2728 0.1274 Uiso 1.00 calc . . . H(19) H -0.8586 0.1376 -0.3064 0.1274 Uiso 1.00 calc . . . H(20) H -0.7683 0.2223 -0.1290 0.1550 Uiso 1.00 calc . . . H(21) H -0.6418 0.1804 -0.0037 0.1550 Uiso 1.00 calc . . . H(22) H -0.8264 0.1787 -0.0363 0.1550 Uiso 1.00 calc . . . H(23) H -0.9601 -0.0314 -0.2639 0.0380 Uiso 1.00 calc . . . H(24) H -0.9332 -0.0947 -0.3454 0.0380 Uiso 1.00 calc . . . H(25) H -0.7051 -0.0889 -0.0426 0.2143 Uiso 1.00 calc . . . H(26) H -0.8568 -0.1264 -0.0960 0.2143 Uiso 1.00 calc . . . H(27) H -0.9494 -0.0647 0.0147 0.3597 Uiso 1.00 calc . . . H(28) H -0.7904 -0.0314 0.0727 0.3597 Uiso 1.00 calc . . . H(29) H -0.6801 -0.0897 0.2772 0.1366 Uiso 1.00 calc . . . H(30) H -0.8463 -0.0564 0.2863 0.1366 Uiso 1.00 calc . . . H(31) H -0.8325 -0.1272 0.2159 0.1366 Uiso 1.00 calc . . . H(32) H -0.426(9) -0.309(3) -0.928(9) 0.13(2) Uiso 1.00 calc . . . H(33) H -0.8457 -0.3876 -1.1404 0.1600 Uiso 1.00 calc . . . H(34) H -0.7616 -0.3808 -0.9440 0.1600 Uiso 1.00 calc . . . H(35) H -0.6532 -0.3302 -1.1611 0.1893 Uiso 1.00 calc . . . H(36) H -0.5758 -0.3927 -1.0886 0.1893 Uiso 1.00 calc . . . H(37) H -0.5557 -0.2333 -0.7946 0.1354 Uiso 1.00 calc . . . H(38) H -0.6359 -0.2368 -0.9911 0.1354 Uiso 1.00 calc . . . H(39) H -0.7539 -0.2865 -0.7813 0.1434 Uiso 1.00 calc . . . H(40) H -0.8290 -0.2254 -0.8626 0.1434 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) 0.049(2) 0.046(2) 0.055(2) -0.008(1) 0.006(2) 0.006(2) O(2) 0.057(2) 0.059(2) 0.118(3) -0.019(2) 0.036(2) 0.001(2) O(3) 0.044(2) 0.036(2) 0.063(2) -0.006(1) 0.020(1) 0.004(1) O(4) 0.062(3) 0.108(4) 0.163(5) -0.002(3) 0.003(3) 0.015(3) N(1) 0.067(3) 0.035(2) 0.091(3) 0.003(2) 0.035(2) 0.005(2) N(2) 0.054(3) 0.133(5) 0.084(4) 0.003(3) 0.018(3) 0.037(3) C(1) 0.042(2) 0.039(3) 0.047(3) -0.008(2) 0.011(2) 0.003(2) C(2) 0.045(3) 0.047(3) 0.042(3) -0.001(2) 0.012(2) 0.011(2) C(3) 0.058(3) 0.044(3) 0.056(3) -0.001(2) 0.020(2) 0.010(2) C(4) 0.065(3) 0.058(4) 0.060(3) 0.012(3) 0.027(3) 0.017(3) C(5) 0.053(3) 0.077(4) 0.068(4) 0.014(3) 0.028(3) 0.019(3) C(6) 0.047(3) 0.066(4) 0.069(3) -0.005(3) 0.019(2) 0.012(3) C(7) 0.044(3) 0.053(3) 0.055(3) 0.000(2) 0.019(2) 0.014(2) C(8) 0.043(3) 0.055(3) 0.059(3) -0.011(2) 0.015(2) 0.009(2) C(9) 0.044(3) 0.045(3) 0.052(3) -0.009(2) 0.014(2) 0.006(2) C(10) 0.047(3) 0.038(3) 0.053(3) -0.009(2) 0.015(2) 0.004(2) C(11) 0.055(3) 0.041(3) 0.076(4) -0.014(2) 0.021(3) 0.003(2) C(12) 0.063(3) 0.039(3) 0.076(4) -0.012(2) 0.023(3) 0.001(2) C(13) 0.057(3) 0.036(3) 0.058(3) -0.007(2) 0.019(2) 0.003(2) C(14) 0.047(3) 0.042(3) 0.055(3) -0.009(2) 0.017(2) 0.001(2) C(15) 0.050(3) 0.034(3) 0.051(3) -0.008(2) 0.016(2) 0.003(2) C(16) 0.038(2) 0.043(3) 0.051(3) -0.006(2) 0.015(2) 0.005(2) C(17) 0.042(2) 0.041(3) 0.051(3) -0.002(2) 0.018(2) 0.008(2) C(18) 0.059(3) 0.063(4) 0.054(3) -0.019(3) 0.006(2) 0.009(3) C(19) 0.077(4) 0.090(5) 0.050(3) -0.022(3) 0.003(3) 0.018(3) C(20) 0.086(4) 0.071(4) 0.063(4) -0.009(3) 0.023(3) 0.027(3) C(21) 0.089(4) 0.050(3) 0.068(4) -0.012(3) 0.032(3) 0.010(3) C(22) 0.070(3) 0.047(3) 0.056(3) -0.011(2) 0.022(3) 0.005(2) C(23) 0.099(4) 0.060(4) 0.090(4) 0.005(3) 0.045(4) 0.010(3) C(24) 0.102(4) 0.058(4) 0.077(4) -0.016(3) 0.031(3) 0.003(3) C(25) 0.156(7) 0.044(4) 0.107(5) -0.013(4) 0.052(5) 0.010(3) C(26) 0.192(9) 0.073(5) 0.131(6) -0.015(5) 0.084(6) 0.012(4) C(27) 0.065(3) 0.049(3) 0.066(3) 0.005(2) 0.027(3) 0.006(2) C(28) 0.222(10) 0.186(9) 0.129(7) 0.147(8) 0.132(7) 0.101(7) C(29) 0.44(2) 0.36(2) 0.100(7) 0.32(2) 0.15(1) 0.109(10) C(30) 0.186(8) 0.094(6) 0.070(4) 0.022(5) 0.036(5) 0.015(4) C(31) 0.083(5) 0.102(6) 0.138(7) -0.002(4) 0.013(5) -0.031(5) C(32) 0.092(5) 0.22(1) 0.077(5) 0.027(6) 0.021(4) -0.012(6) C(33) 0.077(4) 0.100(6) 0.139(6) -0.014(4) 0.016(4) 0.045(5) C(34) 0.076(4) 0.079(5) 0.172(8) -0.004(4) 0.035(5) 0.000(5) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(1) 1.422(5) 1_555 1_555 yes O(2) C(8) 1.218(5) 1_555 1_555 yes O(3) C(15) 1.397(5) 1_555 1_555 yes O(3) C(16) 1.368(5) 1_555 1_555 yes O(4) C(31) 1.382(8) 1_555 1_555 yes O(4) C(34) 1.425(8) 1_555 1_555 yes N(1) C(13) 1.384(6) 1_555 1_555 yes N(1) C(23) 1.459(7) 1_555 1_555 yes N(1) C(27) 1.439(6) 1_555 1_555 yes N(2) C(32) 1.463(9) 1_555 1_555 yes N(2) C(33) 1.475(9) 1_555 1_555 yes C(1) C(2) 1.548(6) 1_555 1_555 yes C(1) C(16) 1.497(6) 1_555 1_555 yes C(1) C(17) 1.536(6) 1_555 1_555 yes C(2) C(3) 1.395(6) 1_555 1_555 yes C(2) C(7) 1.395(6) 1_555 1_555 yes C(3) C(4) 1.374(7) 1_555 1_555 yes C(4) C(5) 1.380(8) 1_555 1_555 yes C(5) C(6) 1.367(8) 1_555 1_555 yes C(6) C(7) 1.400(7) 1_555 1_555 yes C(7) C(8) 1.489(7) 1_555 1_555 yes C(8) C(9) 1.448(6) 1_555 1_555 yes C(9) C(10) 1.450(6) 1_555 1_555 yes C(9) C(16) 1.345(6) 1_555 1_555 yes C(10) C(11) 1.389(6) 1_555 1_555 yes C(10) C(15) 1.384(6) 1_555 1_555 yes C(11) C(12) 1.376(7) 1_555 1_555 yes C(12) C(13) 1.420(7) 1_555 1_555 yes C(13) C(14) 1.395(6) 1_555 1_555 yes C(14) C(15) 1.372(6) 1_555 1_555 yes C(17) C(18) 1.384(6) 1_555 1_555 yes C(17) C(22) 1.370(6) 1_555 1_555 yes C(18) C(19) 1.376(7) 1_555 1_555 yes C(19) C(20) 1.381(8) 1_555 1_555 yes C(20) C(21) 1.372(8) 1_555 1_555 yes C(21) C(22) 1.394(7) 1_555 1_555 yes C(23) C(24) 1.454(8) 1_555 1_555 yes C(24) C(25) 1.505(8) 1_555 1_555 yes C(25) C(26) 1.438(9) 1_555 1_555 yes C(27) C(28) 1.493(9) 1_555 1_555 yes C(28) C(29) 1.053(10) 1_555 1_555 yes C(29) C(30) 1.49(1) 1_555 1_555 yes C(31) C(32) 1.45(1) 1_555 1_555 yes C(33) C(34) 1.454(10) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) O(1) H(1) 101(3) 1_555 1_555 1_555 no C(15) O(3) C(16) 105.5(3) 1_555 1_555 1_555 yes C(31) O(4) C(34) 109.9(5) 1_555 1_555 1_555 yes C(13) N(1) C(23) 122.4(4) 1_555 1_555 1_555 yes C(13) N(1) C(27) 120.1(4) 1_555 1_555 1_555 yes C(23) N(1) C(27) 116.9(4) 1_555 1_555 1_555 yes C(32) N(2) C(33) 108.4(5) 1_555 1_555 1_555 yes C(32) N(2) H(32) 112(3) 1_555 1_555 1_555 no C(33) N(2) H(32) 106(4) 1_555 1_555 1_555 no O(1) C(1) C(2) 111.0(3) 1_555 1_555 1_555 yes O(1) C(1) C(16) 111.3(3) 1_555 1_555 1_555 yes O(1) C(1) C(17) 107.8(3) 1_555 1_555 1_555 yes C(2) C(1) C(16) 108.2(3) 1_555 1_555 1_555 yes C(2) C(1) C(17) 107.8(3) 1_555 1_555 1_555 yes C(16) C(1) C(17) 110.7(3) 1_555 1_555 1_555 yes C(1) C(2) C(3) 117.6(4) 1_555 1_555 1_555 yes C(1) C(2) C(7) 123.2(4) 1_555 1_555 1_555 yes C(3) C(2) C(7) 119.1(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(2) C(3) H(2) 117(3) 1_555 1_555 1_555 no C(4) C(3) H(2) 122(3) 1_555 1_555 1_555 no C(3) C(4) C(5) 120.5(5) 1_555 1_555 1_555 yes C(3) C(4) H(3) 121(2) 1_555 1_555 1_555 no C(5) C(4) H(3) 118(2) 1_555 1_555 1_555 no C(4) C(5) C(6) 119.4(5) 1_555 1_555 1_555 yes C(4) C(5) H(4) 119(3) 1_555 1_555 1_555 no C(6) C(5) H(4) 120(3) 1_555 1_555 1_555 no C(5) C(6) C(7) 121.6(5) 1_555 1_555 1_555 yes C(5) C(6) H(5) 121(3) 1_555 1_555 1_555 no C(7) C(6) H(5) 116(3) 1_555 1_555 1_555 no C(2) C(7) C(6) 118.7(5) 1_555 1_555 1_555 yes C(2) C(7) C(8) 122.3(4) 1_555 1_555 1_555 yes C(6) C(7) C(8) 119.0(4) 1_555 1_555 1_555 yes O(2) C(8) C(7) 121.8(4) 1_555 1_555 1_555 yes O(2) C(8) C(9) 122.9(4) 1_555 1_555 1_555 yes C(7) C(8) C(9) 115.3(4) 1_555 1_555 1_555 yes C(8) C(9) C(10) 131.8(4) 1_555 1_555 1_555 yes C(8) C(9) C(16) 121.7(4) 1_555 1_555 1_555 yes C(10) C(9) C(16) 106.6(4) 1_555 1_555 1_555 yes C(9) C(10) C(11) 137.1(4) 1_555 1_555 1_555 yes C(9) C(10) C(15) 105.4(4) 1_555 1_555 1_555 yes C(11) C(10) C(15) 117.5(4) 1_555 1_555 1_555 yes C(10) C(11) C(12) 118.8(5) 1_555 1_555 1_555 yes C(10) C(11) H(6) 119(3) 1_555 1_555 1_555 no C(12) C(11) H(6) 121(3) 1_555 1_555 1_555 no C(11) C(12) C(13) 122.9(5) 1_555 1_555 1_555 yes C(11) C(12) H(7) 117(3) 1_555 1_555 1_555 no C(13) C(12) H(7) 118(3) 1_555 1_555 1_555 no N(1) C(13) C(12) 120.1(4) 1_555 1_555 1_555 yes N(1) C(13) C(14) 121.8(4) 1_555 1_555 1_555 yes C(12) C(13) C(14) 118.0(4) 1_555 1_555 1_555 yes C(13) C(14) C(15) 117.3(4) 1_555 1_555 1_555 yes C(13) C(14) H(8) 121(2) 1_555 1_555 1_555 no C(15) C(14) H(8) 121(2) 1_555 1_555 1_555 no O(3) C(15) C(10) 110.2(4) 1_555 1_555 1_555 yes O(3) C(15) C(14) 124.3(4) 1_555 1_555 1_555 yes C(10) C(15) C(14) 125.5(4) 1_555 1_555 1_555 yes O(3) C(16) C(1) 119.1(3) 1_555 1_555 1_555 yes O(3) C(16) C(9) 112.3(4) 1_555 1_555 1_555 yes C(1) C(16) C(9) 128.6(4) 1_555 1_555 1_555 yes C(1) C(17) C(18) 120.4(4) 1_555 1_555 1_555 yes C(1) C(17) C(22) 120.6(4) 1_555 1_555 1_555 yes C(18) C(17) C(22) 118.9(4) 1_555 1_555 1_555 yes C(17) C(18) C(19) 120.4(5) 1_555 1_555 1_555 yes C(17) C(18) H(9) 120(2) 1_555 1_555 1_555 no C(19) C(18) H(9) 118(2) 1_555 1_555 1_555 no C(18) C(19) C(20) 120.7(5) 1_555 1_555 1_555 yes C(18) C(19) H(10) 119(3) 1_555 1_555 1_555 no C(20) C(19) H(10) 119(3) 1_555 1_555 1_555 no C(19) C(20) C(21) 119.1(5) 1_555 1_555 1_555 yes C(19) C(20) H(11) 123(3) 1_555 1_555 1_555 no C(21) C(20) H(11) 116(3) 1_555 1_555 1_555 no C(20) C(21) C(22) 120.1(5) 1_555 1_555 1_555 yes C(20) C(21) H(12) 121(3) 1_555 1_555 1_555 no C(22) C(21) H(12) 117(3) 1_555 1_555 1_555 no C(17) C(22) C(21) 120.7(5) 1_555 1_555 1_555 yes C(17) C(22) H(13) 116(2) 1_555 1_555 1_555 no C(21) C(22) H(13) 121(2) 1_555 1_555 1_555 no N(1) C(23) C(24) 117.5(5) 1_555 1_555 1_555 yes N(1) C(23) H(14) 108.4(5) 1_555 1_555 1_555 no N(1) C(23) H(15) 105.8(5) 1_555 1_555 1_555 no C(24) C(23) H(14) 111.0(6) 1_555 1_555 1_555 no C(24) C(23) H(15) 107.8(5) 1_555 1_555 1_555 no H(14) C(23) H(15) 105.7(6) 1_555 1_555 1_555 no C(23) C(24) C(25) 114.4(5) 1_555 1_555 1_555 yes C(23) C(24) H(16) 108.6(5) 1_555 1_555 1_555 no C(23) C(24) H(17) 103.6(5) 1_555 1_555 1_555 no C(25) C(24) H(16) 119.1(5) 1_555 1_555 1_555 no C(25) C(24) H(17) 112.6(6) 1_555 1_555 1_555 no H(16) C(24) H(17) 96.0(5) 1_555 1_555 1_555 no C(24) C(25) C(26) 118.1(6) 1_555 1_555 1_555 yes C(24) C(25) H(18) 111.6(6) 1_555 1_555 1_555 no C(24) C(25) H(19) 105.6(5) 1_555 1_555 1_555 no C(26) C(25) H(18) 111.0(6) 1_555 1_555 1_555 no C(26) C(25) H(19) 102.7(7) 1_555 1_555 1_555 no H(18) C(25) H(19) 106.5(6) 1_555 1_555 1_555 no C(25) C(26) H(20) 110.6(7) 1_555 1_555 1_555 no C(25) C(26) H(21) 103.2(7) 1_555 1_555 1_555 no C(25) C(26) H(22) 110.7(7) 1_555 1_555 1_555 no H(20) C(26) H(21) 109.1(8) 1_555 1_555 1_555 no H(20) C(26) H(22) 114.0(9) 1_555 1_555 1_555 no H(21) C(26) H(22) 108.7(8) 1_555 1_555 1_555 no N(1) C(27) C(28) 113.3(6) 1_555 1_555 1_555 yes N(1) C(27) H(23) 107.8(4) 1_555 1_555 1_555 no N(1) C(27) H(24) 107.8(4) 1_555 1_555 1_555 no C(28) C(27) H(23) 112.7(5) 1_555 1_555 1_555 no C(28) C(27) H(24) 118.5(7) 1_555 1_555 1_555 no H(23) C(27) H(24) 95.0(4) 1_555 1_555 1_555 no C(27) C(28) C(29) 140.0(9) 1_555 1_555 1_555 yes C(27) C(28) H(25) 103.1(6) 1_555 1_555 1_555 no C(27) C(28) H(26) 102.1(9) 1_555 1_555 1_555 no C(29) C(28) H(25) 99(1) 1_555 1_555 1_555 no C(29) C(28) H(26) 101(1) 1_555 1_555 1_555 no H(25) C(28) H(26) 108.3(7) 1_555 1_555 1_555 no C(28) C(29) C(30) 142(1) 1_555 1_555 1_555 yes C(28) C(29) H(27) 98(1) 1_555 1_555 1_555 no C(28) C(29) H(28) 101(1) 1_555 1_555 1_555 no C(30) C(29) H(27) 101(1) 1_555 1_555 1_555 no C(30) C(29) H(28) 99(1) 1_555 1_555 1_555 no H(27) C(29) H(28) 112.5(10) 1_555 1_555 1_555 no C(29) C(30) H(29) 113(1) 1_555 1_555 1_555 no C(29) C(30) H(30) 108.7(7) 1_555 1_555 1_555 no C(29) C(30) H(31) 108(1) 1_555 1_555 1_555 no H(29) C(30) H(30) 113.8(8) 1_555 1_555 1_555 no H(29) C(30) H(31) 108.6(7) 1_555 1_555 1_555 no H(30) C(30) H(31) 103.3(8) 1_555 1_555 1_555 no O(4) C(31) C(32) 112.4(7) 1_555 1_555 1_555 yes O(4) C(31) H(33) 116.6(7) 1_555 1_555 1_555 no O(4) C(31) H(34) 107.0(7) 1_555 1_555 1_555 no C(32) C(31) H(33) 111.1(8) 1_555 1_555 1_555 no C(32) C(31) H(34) 105.0(7) 1_555 1_555 1_555 no H(33) C(31) H(34) 103.6(8) 1_555 1_555 1_555 no N(2) C(32) C(31) 110.4(6) 1_555 1_555 1_555 yes N(2) C(32) H(35) 107.7(9) 1_555 1_555 1_555 no N(2) C(32) H(36) 109.3(7) 1_555 1_555 1_555 no C(31) C(32) H(35) 105.8(7) 1_555 1_555 1_555 no C(31) C(32) H(36) 112(1) 1_555 1_555 1_555 no H(35) C(32) H(36) 111.2(8) 1_555 1_555 1_555 no N(2) C(33) C(34) 108.3(6) 1_555 1_555 1_555 yes N(2) C(33) H(37) 107.9(6) 1_555 1_555 1_555 no N(2) C(33) H(38) 104.2(7) 1_555 1_555 1_555 no C(34) C(33) H(37) 113.3(8) 1_555 1_555 1_555 no C(34) C(33) H(38) 110.8(6) 1_555 1_555 1_555 no H(37) C(33) H(38) 111.9(7) 1_555 1_555 1_555 no O(4) C(34) C(33) 111.3(7) 1_555 1_555 1_555 yes O(4) C(34) H(39) 110.2(7) 1_555 1_555 1_555 no O(4) C(34) H(40) 108.1(7) 1_555 1_555 1_555 no C(33) C(34) H(39) 108.3(7) 1_555 1_555 1_555 no C(33) C(34) H(40) 105.5(7) 1_555 1_555 1_555 no H(39) C(34) H(40) 113.4(9) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ #===============================================END data_ 3c·piperidine _database_code_CSD 172467 #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_formula_sum 'C35 H42 N2 O3 ' _chemical_formula_weight 538.73 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _cell_length_a 8.753(2) _cell_length_b 21.732(3) _cell_length_c 8.355(1) _cell_angle_alpha 97.55(1) _cell_angle_beta 107.03(1) _cell_angle_gamma 81.90(2) _cell_volume 1497.6(5) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.195 _diffrn_radiation_type 'Mo K„a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 21 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 12.2 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_F_000 580.00 _exptl_absorpt_coefficient_mu 0.075 _exptl_crystal_description 'prismatic' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_colour 'yellow' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method „w-2„q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.930 _exptl_absorpt_correction_T_max 0.996 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_radiation_monochromator graphite _diffrn_reflns_number 5653 _reflns_number_total 5273 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.733 _refine_ls_number_reflns 2031 _refine_ls_number_parameters 410 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[„s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 1.4627 _refine_ls_shift/su_mean 0.0078 _refine_diff_density_min -0.30 _refine_diff_density_max 0.38 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.0416(8) 0.1243(4) 0.3832(9) 0.045(2) Uani 1.00 d . . . O(2) O 0.4771(9) 0.2895(4) 0.5996(10) 0.067(3) Uani 1.00 d . . . O(3) O -0.0151(7) 0.2384(3) 0.5917(8) 0.039(2) Uani 1.00 d . . . N(1) N -0.2389(10) 0.4500(4) 0.726(1) 0.046(3) Uani 1.00 d . . . N(2) N 0.991(1) 0.1880(8) 0.104(2) 0.099(5) Uani 1.00 d . . . C(1) C 0.170(1) 0.1479(4) 0.521(1) 0.039(3) Uani 1.00 d . . . C(2) C 0.331(1) 0.1376(4) 0.477(1) 0.037(3) Uani 1.00 d . . . C(3) C 0.380(1) 0.0774(5) 0.416(1) 0.048(4) Uani 1.00 d . . . C(4) C 0.528(1) 0.0651(6) 0.386(1) 0.059(4) Uani 1.00 d . . . C(5) C 0.627(2) 0.1103(7) 0.419(2) 0.064(5) Uani 1.00 d . . . C(6) C 0.582(1) 0.1700(6) 0.477(1) 0.055(4) Uani 1.00 d . . . C(7) C 0.432(1) 0.1824(5) 0.508(1) 0.041(3) Uani 1.00 d . . . C(8) C 0.384(1) 0.2487(5) 0.569(1) 0.046(3) Uani 1.00 d . . . C(9) C 0.224(1) 0.2619(4) 0.587(1) 0.037(3) Uani 1.00 d . . . C(10) C 0.133(1) 0.3189(4) 0.631(1) 0.036(3) Uani 1.00 d . . . C(11) C 0.150(1) 0.3808(5) 0.664(1) 0.052(4) Uani 1.00 d . . . C(12) C 0.028(1) 0.4243(5) 0.698(1) 0.051(4) Uani 1.00 d . . . C(13) C -0.123(1) 0.4052(5) 0.691(1) 0.041(3) Uani 1.00 d . . . C(14) C -0.141(1) 0.3426(5) 0.659(1) 0.050(4) Uani 1.00 d . . . C(15) C -0.015(1) 0.3012(4) 0.628(1) 0.039(3) Uani 1.00 d . . . C(16) C 0.130(1) 0.2157(4) 0.564(1) 0.033(3) Uani 1.00 d . . . C(17) C 0.183(1) 0.1095(4) 0.670(1) 0.038(3) Uani 1.00 d . . . C(18) C 0.293(1) 0.1271(6) 0.825(1) 0.066(4) Uani 1.00 d . . . C(19) C 0.315(2) 0.0889(7) 0.954(1) 0.082(5) Uani 1.00 d . . . C(20) C 0.238(2) 0.0401(6) 0.937(2) 0.069(5) Uani 1.00 d . . . C(21) C 0.130(2) 0.0230(6) 0.788(2) 0.063(4) Uani 1.00 d . . . C(22) C 0.105(2) 0.0590(6) 0.654(2) 0.052(4) Uani 1.00 d . . . C(23) C -0.257(1) 0.5137(6) 0.679(1) 0.068(4) Uani 1.00 d . . . C(24) C -0.242(1) 0.5634(6) 0.816(1) 0.070(5) Uani 1.00 d . . . C(25) C -0.259(2) 0.6288(5) 0.760(2) 0.084(5) Uani 1.00 d . . . C(26) C -0.275(2) 0.6781(7) 0.886(2) 0.113(7) Uani 1.00 d . . . C(27) C -0.382(1) 0.4298(5) 0.754(1) 0.054(4) Uani 1.00 d . . . C(28) C -0.354(1) 0.4022(5) 0.921(1) 0.058(4) Uani 1.00 d . . . C(29) C -0.280(1) 0.4467(6) 1.069(2) 0.071(4) Uani 1.00 d . . . C(30) C -0.257(2) 0.4215(7) 1.241(2) 0.091(5) Uani 1.00 d . . . C(31) C 0.911(2) 0.2500(7) 0.146(2) 0.091(6) Uani 1.00 d . . . C(32) C 0.755(2) 0.2413(6) 0.173(2) 0.086(5) Uani 1.00 d . . . C(33) C 0.650(2) 0.2072(7) 0.033(2) 0.106(6) Uani 1.00 d . . . C(34) C 0.732(2) 0.1470(7) -0.022(2) 0.101(6) Uani 1.00 d . . . C(35) C 0.887(2) 0.156(1) -0.053(2) 0.102(7) Uani 1.00 d . . . H(1) H 0.067(9) 0.092(4) 0.359(10) 0.01(3) Uiso 1.00 calc . . . H(2) H 0.97(1) 0.205(6) 0.01(2) 0.07(4) Uiso 1.00 calc . . . H(3) H 0.30(1) 0.042(4) 0.40(1) 0.05(3) Uiso 1.00 calc . . . H(4) H 0.56(1) 0.020(5) 0.35(1) 0.07(4) Uiso 1.00 calc . . . H(5) H 0.701(9) 0.102(4) 0.408(10) 0.01(3) Uiso 1.00 calc . . . H(6) H 0.66(1) 0.212(4) 0.52(1) 0.06(3) Uiso 1.00 calc . . . H(7) H 0.2486 0.3948 0.6642 0.0621 Uiso 1.00 calc . . . H(8) H 0.06(1) 0.476(5) 0.69(1) 0.09(4) Uiso 1.00 calc . . . H(9) H -0.2384 0.3279 0.6575 0.0595 Uiso 1.00 calc . . . H(10) H 0.35(1) 0.173(5) 0.84(1) 0.07(3) Uiso 1.00 calc . . . H(11) H 0.3904 0.0989 1.0599 0.0990 Uiso 1.00 calc . . . H(12) H 0.2573 0.0161 1.0300 0.0845 Uiso 1.00 calc . . . H(13) H 0.08(2) -0.016(6) 0.80(2) 0.13(5) Uiso 1.00 calc . . . H(14) H 0.05(1) 0.049(4) 0.57(1) 0.03(3) Uiso 1.00 calc . . . H(15) H -0.1768 0.5163 0.6248 0.0825 Uiso 1.00 calc . . . H(16) H -0.3603 0.5210 0.6020 0.0825 Uiso 1.00 calc . . . H(17) H -0.1388 0.5568 0.8938 0.0840 Uiso 1.00 calc . . . H(18) H -0.3224 0.5617 0.8706 0.0840 Uiso 1.00 calc . . . H(19) H -0.1708 0.6331 0.7205 0.1028 Uiso 1.00 calc . . . H(20) H -0.3560 0.6326 0.6646 0.1028 Uiso 1.00 calc . . . H(21) H -0.1720 0.6839 0.9579 0.1360 Uiso 1.00 calc . . . H(22) H -0.3229 0.7153 0.8346 0.1360 Uiso 1.00 calc . . . H(23) H -0.3414 0.6669 0.9469 0.1360 Uiso 1.00 calc . . . H(24) H -0.4225 0.3990 0.6658 0.0659 Uiso 1.00 calc . . . H(25) H -0.4603 0.4650 0.7507 0.0659 Uiso 1.00 calc . . . H(26) H -0.2842 0.3646 0.9212 0.0697 Uiso 1.00 calc . . . H(27) H -0.4545 0.3934 0.9297 0.0697 Uiso 1.00 calc . . . H(28) H -0.1784 0.4539 1.0613 0.0859 Uiso 1.00 calc . . . H(29) H -0.3486 0.4848 1.0648 0.0859 Uiso 1.00 calc . . . H(30) H -0.2107 0.4512 1.3287 0.1119 Uiso 1.00 calc . . . H(31) H -0.3580 0.4139 1.2501 0.1119 Uiso 1.00 calc . . . H(32) H -0.1874 0.3835 1.2472 0.1119 Uiso 1.00 calc . . . H(33) H 0.8895 0.2761 0.0519 0.1107 Uiso 1.00 calc . . . H(34) H 0.9757 0.2722 0.2416 0.1107 Uiso 1.00 calc . . . H(35) H 0.7008 0.2812 0.1942 0.1028 Uiso 1.00 calc . . . H(36) H 0.7806 0.2190 0.2688 0.1028 Uiso 1.00 calc . . . H(37) H 0.6132 0.2325 -0.0576 0.1293 Uiso 1.00 calc . . . H(38) H 0.5620 0.1989 0.0682 0.1293 Uiso 1.00 calc . . . H(39) H 0.7537 0.1193 0.0618 0.1215 Uiso 1.00 calc . . . H(40) H 0.6637 0.1298 -0.1238 0.1215 Uiso 1.00 calc . . . H(41) H 0.99(2) 0.131(7) -0.06(2) 0.15(7) Uiso 1.00 calc . . . H(42) H 0.84(1) 0.190(5) -0.15(1) 0.07(4) 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) 0.041(4) 0.027(5) 0.054(5) -0.001(4) -0.005(4) -0.003(4) O(2) 0.046(5) 0.073(6) 0.088(6) -0.012(4) 0.024(4) 0.008(5) O(3) 0.044(4) 0.031(4) 0.042(4) -0.007(3) 0.012(3) 0.000(3) N(1) 0.055(6) 0.028(5) 0.062(6) -0.003(4) 0.030(5) 0.006(4) N(2) 0.066(8) 0.15(1) 0.08(1) 0.007(8) 0.017(7) 0.05(1) C(1) 0.035(6) 0.044(7) 0.036(6) -0.001(5) 0.007(5) 0.004(5) C(2) 0.040(6) 0.034(6) 0.041(6) -0.001(5) 0.014(5) 0.014(5) C(3) 0.048(7) 0.055(8) 0.045(7) 0.001(6) 0.017(6) 0.016(6) C(4) 0.069(9) 0.062(9) 0.055(8) 0.012(8) 0.033(7) 0.023(7) C(5) 0.037(8) 0.09(1) 0.078(10) 0.007(8) 0.033(7) 0.030(8) C(6) 0.048(7) 0.060(9) 0.048(7) 0.002(6) 0.008(6) -0.003(6) C(7) 0.038(6) 0.050(7) 0.035(6) 0.003(5) 0.010(5) 0.006(5) C(8) 0.041(6) 0.058(8) 0.043(7) -0.015(6) 0.010(5) 0.015(6) C(9) 0.041(6) 0.033(6) 0.036(6) -0.006(5) 0.007(5) 0.004(5) C(10) 0.036(6) 0.030(6) 0.040(6) -0.016(5) 0.005(5) 0.002(5) C(11) 0.045(7) 0.065(9) 0.051(7) -0.004(6) 0.018(6) 0.018(6) C(12) 0.065(8) 0.049(8) 0.035(6) -0.006(6) 0.008(5) 0.001(5) C(13) 0.054(7) 0.025(6) 0.043(7) -0.008(5) 0.014(5) -0.001(5) C(14) 0.045(7) 0.065(9) 0.038(6) 0.009(6) 0.018(5) 0.008(6) C(15) 0.057(7) 0.023(6) 0.037(6) -0.007(5) 0.014(5) 0.001(4) C(16) 0.035(6) 0.031(6) 0.038(6) -0.005(5) 0.012(5) 0.007(4) C(17) 0.043(6) 0.033(6) 0.037(6) 0.003(5) 0.011(5) 0.007(5) C(18) 0.061(8) 0.09(1) 0.044(7) -0.011(7) -0.003(6) 0.024(7) C(19) 0.075(9) 0.12(1) 0.045(8) -0.041(9) -0.012(7) 0.033(8) C(20) 0.079(9) 0.08(1) 0.056(9) -0.012(8) 0.019(7) 0.028(7) C(21) 0.10(1) 0.045(8) 0.057(9) -0.010(7) 0.032(8) 0.007(6) C(22) 0.065(9) 0.045(8) 0.048(9) -0.008(6) 0.013(7) 0.009(6) C(23) 0.087(9) 0.055(8) 0.064(9) -0.004(7) 0.027(7) -0.003(6) C(24) 0.091(10) 0.063(9) 0.064(9) -0.019(7) 0.034(7) -0.004(7) C(25) 0.16(1) 0.034(7) 0.073(10) -0.017(8) 0.046(9) 0.007(7) C(26) 0.15(2) 0.08(1) 0.13(1) 0.01(1) 0.08(1) 0.04(1) C(27) 0.066(8) 0.046(7) 0.050(7) 0.010(6) 0.023(6) 0.000(5) C(28) 0.062(8) 0.055(8) 0.063(8) -0.002(6) 0.027(6) 0.007(6) C(29) 0.078(9) 0.077(9) 0.054(8) 0.001(7) 0.015(7) 0.008(7) C(30) 0.13(1) 0.09(1) 0.053(8) 0.007(9) 0.026(8) 0.010(7) C(31) 0.08(1) 0.09(1) 0.10(1) -0.003(9) 0.021(9) 0.033(9) C(32) 0.070(9) 0.07(1) 0.11(1) -0.011(8) 0.025(9) -0.003(8) C(33) 0.08(1) 0.10(1) 0.11(1) -0.021(9) -0.002(9) -0.02(1) C(34) 0.09(1) 0.10(1) 0.08(1) 0.012(9) 0.005(9) -0.012(9) C(35) 0.07(1) 0.15(2) 0.08(1) 0.00(1) 0.023(10) -0.01(1) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(1) 1.45(1) 1_555 1_555 yes O(2) C(8) 1.24(1) 1_555 1_555 yes O(3) C(15) 1.36(1) 1_555 1_555 yes O(3) C(16) 1.37(1) 1_555 1_555 yes N(1) C(13) 1.37(1) 1_555 1_555 yes N(1) C(23) 1.46(1) 1_555 1_555 yes N(1) C(27) 1.48(1) 1_555 1_555 yes N(2) C(31) 1.48(2) 1_555 1_555 yes N(2) C(35) 1.51(2) 1_555 1_555 yes C(1) C(2) 1.54(1) 1_555 1_555 yes C(1) C(16) 1.48(1) 1_555 1_555 yes C(1) C(17) 1.55(1) 1_555 1_555 yes C(2) C(3) 1.40(1) 1_555 1_555 yes C(2) C(7) 1.35(1) 1_555 1_555 yes C(3) C(4) 1.37(1) 1_555 1_555 yes C(4) C(5) 1.35(2) 1_555 1_555 yes C(5) C(6) 1.37(2) 1_555 1_555 yes C(6) C(7) 1.40(1) 1_555 1_555 yes C(7) C(8) 1.51(1) 1_555 1_555 yes C(8) C(9) 1.43(1) 1_555 1_555 yes C(9) C(10) 1.44(1) 1_555 1_555 yes C(9) C(16) 1.34(1) 1_555 1_555 yes C(10) C(11) 1.36(1) 1_555 1_555 yes C(10) C(15) 1.40(1) 1_555 1_555 yes C(11) C(12) 1.40(1) 1_555 1_555 yes C(12) C(13) 1.43(1) 1_555 1_555 yes C(13) C(14) 1.37(1) 1_555 1_555 yes C(14) C(15) 1.38(1) 1_555 1_555 yes C(17) C(18) 1.41(1) 1_555 1_555 yes C(17) C(22) 1.35(1) 1_555 1_555 yes C(18) C(19) 1.40(2) 1_555 1_555 yes C(19) C(20) 1.31(2) 1_555 1_555 yes C(20) C(21) 1.37(2) 1_555 1_555 yes C(21) C(22) 1.39(2) 1_555 1_555 yes C(23) C(24) 1.46(1) 1_555 1_555 yes C(24) C(25) 1.53(2) 1_555 1_555 yes C(25) C(26) 1.42(2) 1_555 1_555 yes C(27) C(28) 1.53(1) 1_555 1_555 yes C(28) C(29) 1.51(2) 1_555 1_555 yes C(29) C(30) 1.55(2) 1_555 1_555 yes C(31) C(32) 1.49(2) 1_555 1_555 yes C(32) C(33) 1.45(2) 1_555 1_555 yes C(33) C(34) 1.49(2) 1_555 1_555 yes C(34) C(35) 1.49(2) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) O(1) H(1) 108(6) 1_555 1_555 1_555 no C(15) O(3) C(16) 107.2(7) 1_555 1_555 1_555 yes C(13) N(1) C(23) 122.3(9) 1_555 1_555 1_555 yes C(13) N(1) C(27) 118.4(8) 1_555 1_555 1_555 yes C(23) N(1) C(27) 115.8(8) 1_555 1_555 1_555 yes C(31) N(2) C(35) 110(1) 1_555 1_555 1_555 yes C(31) N(2) H(2) 79(8) 1_555 1_555 1_555 no C(35) N(2) H(2) 63(8) 1_555 1_555 1_555 no O(1) C(1) C(2) 111.3(8) 1_555 1_555 1_555 yes O(1) C(1) C(16) 110.0(7) 1_555 1_555 1_555 yes O(1) C(1) C(17) 105.6(8) 1_555 1_555 1_555 yes C(2) C(1) C(16) 109.1(8) 1_555 1_555 1_555 yes C(2) C(1) C(17) 109.2(7) 1_555 1_555 1_555 yes C(16) C(1) C(17) 111.7(8) 1_555 1_555 1_555 yes C(1) C(2) C(3) 117.5(9) 1_555 1_555 1_555 yes C(1) C(2) C(7) 123.0(9) 1_555 1_555 1_555 yes C(3) C(2) C(7) 119.2(9) 1_555 1_555 1_555 yes C(2) C(3) C(4) 119(1) 1_555 1_555 1_555 yes C(2) C(3) H(3) 118(4) 1_555 1_555 1_555 no C(4) C(3) H(3) 122(4) 1_555 1_555 1_555 no C(3) C(4) C(5) 120(1) 1_555 1_555 1_555 yes C(3) C(4) H(4) 113(6) 1_555 1_555 1_555 no C(5) C(4) H(4) 126(6) 1_555 1_555 1_555 no C(4) C(5) C(6) 122(1) 1_555 1_555 1_555 yes C(4) C(5) H(5) 116(7) 1_555 1_555 1_555 no C(6) C(5) H(5) 121(7) 1_555 1_555 1_555 no C(5) C(6) C(7) 117(1) 1_555 1_555 1_555 yes C(5) C(6) H(6) 129(4) 1_555 1_555 1_555 no C(7) C(6) H(6) 112(4) 1_555 1_555 1_555 no C(2) C(7) C(6) 121.4(10) 1_555 1_555 1_555 yes C(2) C(7) C(8) 121.7(9) 1_555 1_555 1_555 yes C(6) C(7) C(8) 116.8(10) 1_555 1_555 1_555 yes O(2) C(8) C(7) 121.5(9) 1_555 1_555 1_555 yes O(2) C(8) C(9) 122(1) 1_555 1_555 1_555 yes C(7) C(8) C(9) 116.2(9) 1_555 1_555 1_555 yes C(8) C(9) C(10) 132.3(9) 1_555 1_555 1_555 yes C(8) C(9) C(16) 120.4(9) 1_555 1_555 1_555 yes C(10) C(9) C(16) 107.3(8) 1_555 1_555 1_555 yes C(9) C(10) C(11) 138.5(9) 1_555 1_555 1_555 yes C(9) C(10) C(15) 104.8(8) 1_555 1_555 1_555 yes C(11) C(10) C(15) 116.5(9) 1_555 1_555 1_555 yes C(10) C(11) C(12) 121.8(10) 1_555 1_555 1_555 yes C(10) C(11) H(7) 118(1) 1_555 1_555 1_555 no C(12) C(11) H(7) 119(1) 1_555 1_555 1_555 no C(11) C(12) C(13) 120(1) 1_555 1_555 1_555 yes C(11) C(12) H(8) 110(5) 1_555 1_555 1_555 no C(13) C(12) H(8) 126(5) 1_555 1_555 1_555 no N(1) C(13) C(12) 117.9(9) 1_555 1_555 1_555 yes N(1) C(13) C(14) 124.2(9) 1_555 1_555 1_555 yes C(12) C(13) C(14) 117.8(9) 1_555 1_555 1_555 yes C(13) C(14) C(15) 119.5(10) 1_555 1_555 1_555 yes C(13) C(14) H(9) 120.2(10) 1_555 1_555 1_555 no C(15) C(14) H(9) 120(1) 1_555 1_555 1_555 no O(3) C(15) C(10) 109.9(8) 1_555 1_555 1_555 yes O(3) C(15) C(14) 126.3(9) 1_555 1_555 1_555 yes C(10) C(15) C(14) 123.8(9) 1_555 1_555 1_555 yes O(3) C(16) C(1) 121.0(7) 1_555 1_555 1_555 yes O(3) C(16) C(9) 110.7(8) 1_555 1_555 1_555 yes C(1) C(16) C(9) 128.3(9) 1_555 1_555 1_555 yes C(1) C(17) C(18) 116.6(9) 1_555 1_555 1_555 yes C(1) C(17) C(22) 123.6(9) 1_555 1_555 1_555 yes C(18) C(17) C(22) 119(1) 1_555 1_555 1_555 yes C(17) C(18) C(19) 116(1) 1_555 1_555 1_555 yes C(17) C(18) H(10) 117(4) 1_555 1_555 1_555 no C(19) C(18) H(10) 125(4) 1_555 1_555 1_555 no C(18) C(19) C(20) 123(1) 1_555 1_555 1_555 yes C(18) C(19) H(11) 118(1) 1_555 1_555 1_555 no C(20) C(19) H(11) 118(1) 1_555 1_555 1_555 no C(19) C(20) C(21) 120(1) 1_555 1_555 1_555 yes C(19) C(20) H(12) 119(1) 1_555 1_555 1_555 no C(21) C(20) H(12) 119(1) 1_555 1_555 1_555 no C(20) C(21) C(22) 118(1) 1_555 1_555 1_555 yes C(20) C(21) H(13) 108(7) 1_555 1_555 1_555 no C(22) C(21) H(13) 133(7) 1_555 1_555 1_555 no C(17) C(22) C(21) 121(1) 1_555 1_555 1_555 yes C(17) C(22) H(14) 118(7) 1_555 1_555 1_555 no C(21) C(22) H(14) 119(7) 1_555 1_555 1_555 no N(1) C(23) C(24) 116(1) 1_555 1_555 1_555 yes N(1) C(23) H(15) 107(1) 1_555 1_555 1_555 no N(1) C(23) H(16) 107(1) 1_555 1_555 1_555 no C(24) C(23) H(15) 107(1) 1_555 1_555 1_555 no C(24) C(23) H(16) 107(1) 1_555 1_555 1_555 no H(15) C(23) H(16) 109(1) 1_555 1_555 1_555 no C(23) C(24) C(25) 113(1) 1_555 1_555 1_555 yes C(23) C(24) H(17) 108(1) 1_555 1_555 1_555 no C(23) C(24) H(18) 108(1) 1_555 1_555 1_555 no C(25) C(24) H(17) 107(1) 1_555 1_555 1_555 no C(25) C(24) H(18) 108(1) 1_555 1_555 1_555 no H(17) C(24) H(18) 109(1) 1_555 1_555 1_555 no C(24) C(25) C(26) 114(1) 1_555 1_555 1_555 yes C(24) C(25) H(19) 109(1) 1_555 1_555 1_555 no C(24) C(25) H(20) 107(1) 1_555 1_555 1_555 no C(26) C(25) H(19) 109(1) 1_555 1_555 1_555 no C(26) C(25) H(20) 107(1) 1_555 1_555 1_555 no H(19) C(25) H(20) 107(1) 1_555 1_555 1_555 no C(25) C(26) H(21) 108(1) 1_555 1_555 1_555 no C(25) C(26) H(22) 109(1) 1_555 1_555 1_555 no C(25) C(26) H(23) 108(1) 1_555 1_555 1_555 no H(21) C(26) H(22) 110(1) 1_555 1_555 1_555 no H(21) C(26) H(23) 110(1) 1_555 1_555 1_555 no H(22) C(26) H(23) 109(1) 1_555 1_555 1_555 no N(1) C(27) C(28) 115.6(9) 1_555 1_555 1_555 yes N(1) C(27) H(24) 107.9(9) 1_555 1_555 1_555 no N(1) C(27) H(25) 107.9(10) 1_555 1_555 1_555 no C(28) C(27) H(24) 107(1) 1_555 1_555 1_555 no C(28) C(27) H(25) 107.9(9) 1_555 1_555 1_555 no H(24) C(27) H(25) 109(1) 1_555 1_555 1_555 no C(27) C(28) C(29) 111.6(10) 1_555 1_555 1_555 yes C(27) C(28) H(26) 108.7(10) 1_555 1_555 1_555 no C(27) C(28) H(27) 108(1) 1_555 1_555 1_555 no C(29) C(28) H(26) 109(1) 1_555 1_555 1_555 no C(29) C(28) H(27) 109.1(10) 1_555 1_555 1_555 no H(26) C(28) H(27) 109(1) 1_555 1_555 1_555 no C(28) C(29) C(30) 113(1) 1_555 1_555 1_555 yes C(28) C(29) H(28) 108(1) 1_555 1_555 1_555 no C(28) C(29) H(29) 108(1) 1_555 1_555 1_555 no C(30) C(29) H(28) 108(1) 1_555 1_555 1_555 no C(30) C(29) H(29) 108(1) 1_555 1_555 1_555 no H(28) C(29) H(29) 109(1) 1_555 1_555 1_555 no C(29) C(30) H(30) 109(1) 1_555 1_555 1_555 no C(29) C(30) H(31) 109(1) 1_555 1_555 1_555 no C(29) C(30) H(32) 109(1) 1_555 1_555 1_555 no H(30) C(30) H(31) 110(1) 1_555 1_555 1_555 no H(30) C(30) H(32) 109(1) 1_555 1_555 1_555 no H(31) C(30) H(32) 109(1) 1_555 1_555 1_555 no N(2) C(31) C(32) 108(1) 1_555 1_555 1_555 yes N(2) C(31) H(33) 110(1) 1_555 1_555 1_555 no N(2) C(31) H(34) 112(1) 1_555 1_555 1_555 no C(32) C(31) H(33) 108(1) 1_555 1_555 1_555 no C(32) C(31) H(34) 110(1) 1_555 1_555 1_555 no H(33) C(31) H(34) 106(1) 1_555 1_555 1_555 no C(31) C(32) C(33) 114(1) 1_555 1_555 1_555 yes C(31) C(32) H(35) 108(1) 1_555 1_555 1_555 no C(31) C(32) H(36) 106(1) 1_555 1_555 1_555 no C(33) C(32) H(35) 108(1) 1_555 1_555 1_555 no C(33) C(32) H(36) 109(1) 1_555 1_555 1_555 no H(35) C(32) H(36) 109(1) 1_555 1_555 1_555 no C(32) C(33) C(34) 112(1) 1_555 1_555 1_555 yes C(32) C(33) H(37) 108(1) 1_555 1_555 1_555 no C(32) C(33) H(38) 107(1) 1_555 1_555 1_555 no C(34) C(33) H(37) 109(1) 1_555 1_555 1_555 no C(34) C(33) H(38) 108(1) 1_555 1_555 1_555 no H(37) C(33) H(38) 109(1) 1_555 1_555 1_555 no C(33) C(34) C(35) 111(1) 1_555 1_555 1_555 yes C(33) C(34) H(39) 109(1) 1_555 1_555 1_555 no C(33) C(34) H(40) 108(1) 1_555 1_555 1_555 no C(35) C(34) H(39) 108(1) 1_555 1_555 1_555 no C(35) C(34) H(40) 108(1) 1_555 1_555 1_555 no H(39) C(34) H(40) 109(1) 1_555 1_555 1_555 no N(2) C(35) C(34) 108(1) 1_555 1_555 1_555 yes N(2) C(35) H(41) 85(9) 1_555 1_555 1_555 no N(2) C(35) H(42) 107(6) 1_555 1_555 1_555 no C(34) C(35) H(41) 139(9) 1_555 1_555 1_555 no C(34) C(35) H(42) 98(5) 1_555 1_555 1_555 no H(41) C(35) H(42) 112(10) 1_555 1_555 1_555 no #--------------------------------------------------------------- #===============================================END