#------------------------------------------------------------------------------ #$Date: 2011-09-17 22:27:16 +0200 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003269.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003269 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 458 _journal_page_last 461 _publ_section_title ; Hindered Cavity-shape N-Oxides ; _chemical_formula_moiety 'C17 H13 N1 O2' _chemical_formula_sum 'C17 H13 N O2' _[local]_cod_chemical_formula_sum_orig 'C17 H13 N1 O2' _chemical_formula_weight 263.28 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _[local]_cod_cif_authors_sg_H-M 'P 21/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 14.257(2) _cell_length_b 7.2001(8) _cell_length_c 12.871(1) _cell_angle_alpha 90.00 _cell_angle_beta 108.88(1) _cell_angle_gamma 90.00 _cell_volume 1250.1(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _cell_measurement_reflns_used 15 _cell_measurement_theta_min 21.60 _cell_measurement_theta_max 44.15 _exptl_absorpt_coefficient_mu 0.742 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_colour colorless _chemical_compound_source ? _diffrn_measurement_device 'Syntex P2~1~' _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 1653 _reflns_number_total 1653 _reflns_number_observed 1258 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_theta_max 57.35 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.5 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0421 _refine_ls_wR_factor_obs 0.1112 _refine_ls_wR_factor_all 0.1244 _refine_ls_goodness_of_fit_obs 1.159 _refine_ls_goodness_of_fit_all 1.109 _refine_ls_number_reflns 1653 _refine_ls_number_parameters 186 _refine_ls_hydrogen_treatment ; noref except for H1 for which all parameters refined ; _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0658P)^2^ + 0.3321P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.132 _refine_diff_density_min -0.150 _refine_ls_extinction_method SHELXL93 _refine_ls_extinction_coef 0.0136(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0181 0.009 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0311 0.018 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0492 0.032 _computing_data_collection ; Stereochemical Workstation Operation Manual (Siemens, 1989) ; loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 1 0.2861(2) 0.0725(3) 0.6711(2) 0.0583(6) O1 1 0.37884(13) 0.0199(2) 0.7300(2) 0.0772(6) H1 1 0.3847(25) 0.0355(45) 0.8107(30) 0.119(12) C2 1 0.2399(2) -0.0158(3) 0.5709(2) 0.0683(7) H2 1 0.2728(2) -0.1106(3) 0.5478(2) 0.082 C3 1 0.1475(2) 0.0349(4) 0.5068(2) 0.0768(8) H3 1 0.1168(2) -0.0291(4) 0.4419(2) 0.092 C4 1 0.0989(2) 0.1800(4) 0.5369(2) 0.0692(7) H4 1 0.0360(2) 0.2141(4) 0.4918(2) 0.083 C4a 1 0.1428(2) 0.2751(3) 0.6335(2) 0.0558(6) C5 1 0.0971(2) 0.4481(3) 0.6615(2) 0.0654(7) H5a 1 0.0664(2) 0.4206(3) 0.7168(2) 0.078 H5b 1 0.0465(2) 0.4949(3) 0.5967(2) 0.078 C6 1 0.1782(2) 0.5933(3) 0.7048(2) 0.0613(7) H6a 1 0.2098(2) 0.6194(3) 0.6501(2) 0.074 H6b 1 0.1498(2) 0.7078(3) 0.7210(2) 0.074 C6a 1 0.2529(2) 0.5186(3) 0.8073(2) 0.0502(6) C7 1 0.2940(2) 0.6235(3) 0.8987(2) 0.0545(6) H7 1 0.2779(2) 0.7488(3) 0.8979(2) 0.065 C7a 1 0.3607(2) 0.5451(3) 0.9946(2) 0.0514(6) C8 1 0.4084(2) 0.6470(3) 1.0902(2) 0.0628(7) H8 1 0.3968(2) 0.7739(3) 1.0918(2) 0.075 C9 1 0.4717(2) 0.5623(4) 1.1808(2) 0.0678(7) H9 1 0.5022(2) 0.6316(4) 1.2437(2) 0.081 C10 1 0.4908(2) 0.3719(4) 1.1798(2) 0.0635(7) H10 1 0.5341(2) 0.3157(4) 1.2420(2) 0.076 C11 1 0.4465(2) 0.2675(3) 1.0882(2) 0.0571(6) H11 1 0.4591(2) 0.1408(3) 1.0876(2) 0.069 C11a 1 0.38195(15) 0.3546(3) 0.9957(2) 0.0484(6) N12 1 0.33687(13) 0.2498(2) 0.90075(14) 0.0497(5) O12 1 0.35461(12) 0.0677(2) 0.90806(14) 0.0652(5) C12a 1 0.27791(15) 0.3271(3) 0.8065(2) 0.0479(6) C12b 1 0.2362(2) 0.2177(3) 0.7052(2) 0.0499(6) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C1 0.0637(15) 0.0002(11) 0.0333(12) 0.0471(13) 0.0012(11) 0.072(2) O1 0.0664(12) 0.0134(9) 0.0315(11) 0.0675(12) -0.0122(10) 0.101(2) C2 0.097(2) -0.0073(13) 0.043(2) 0.0487(14) -0.0069(13) 0.071(2) C3 0.103(2) -0.017(2) 0.024(2) 0.065(2) -0.0008(14) 0.060(2) C4 0.074(2) -0.0037(14) 0.0140(13) 0.069(2) 0.0121(13) 0.0598(15) C4a 0.0618(14) -0.0010(11) 0.0229(11) 0.0552(14) 0.0090(11) 0.0534(13) C5 0.0626(15) 0.0180(13) 0.0154(12) 0.072(2) 0.0150(12) 0.0587(15) C6 0.076(2) 0.0145(12) 0.0308(13) 0.0495(13) 0.0142(11) 0.0648(15) C6a 0.0518(13) 0.0049(10) 0.0295(11) 0.0426(12) 0.0063(11) 0.0639(14) C7 0.0612(14) 0.0064(10) 0.0349(12) 0.0378(12) 0.0018(11) 0.074(2) C7a 0.0508(12) -0.0006(10) 0.0271(11) 0.0491(13) -0.0033(11) 0.0608(14) C8 0.071(2) -0.0019(12) 0.0337(13) 0.0535(14) -0.0146(13) 0.071(2) C9 0.065(2) -0.0043(13) 0.0235(13) 0.077(2) -0.0143(13) 0.063(2) C10 0.0560(14) 0.0012(12) 0.0184(11) 0.074(2) 0.0021(13) 0.0601(14) C11 0.0519(13) 0.0012(11) 0.0191(11) 0.0552(14) 0.0015(12) 0.0645(15) C11a 0.0435(12) -0.0016(9) 0.0198(10) 0.0467(13) -0.0022(10) 0.0575(13) N12 0.0469(10) 0.0028(7) 0.0194(9) 0.0378(10) 0.0021(8) 0.0652(12) O12 0.0684(10) 0.0083(7) 0.0104(9) 0.0385(9) 0.0004(7) 0.0791(12) C12a 0.0437(11) 0.0032(9) 0.0228(10) 0.0438(12) 0.0045(11) 0.0603(13) C12b 0.0512(13) -0.0024(10) 0.0225(11) 0.0445(13) 0.0038(10) 0.0574(13) _cod_database_code 2003269