#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003270.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_2003270 _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 'C18 H15 N O2' _chemical_formula_sum 'C18 H15 N O2' _chemical_formula_weight 277.31 _space_group_IT_number 7 _symmetry_space_group_name_Hall 'P -2yac' _symmetry_space_group_name_H-M 'P 1 n 1' _[local]_cod_cif_authors_sg_H-M 'P n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 16.092(2) _cell_length_b 7.9060(10) _cell_length_c 11.8890(10) _cell_angle_alpha 90.00 _cell_angle_beta 115.200(10) _cell_angle_gamma 90.00 _cell_volume 1368.6(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.346 _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 8.25 _cell_measurement_theta_max 43.35 _exptl_absorpt_coefficient_mu 0.704 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _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 1935 _reflns_number_total 1865 _reflns_number_observed 1768 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_theta_max 57.32 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.2 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0553 _refine_ls_wR_factor_obs 0.1412 _refine_ls_wR_factor_all 0.1450 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_goodness_of_fit_all 1.072 _refine_ls_number_reflns 1865 _refine_ls_number_parameters 382 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.1141P)^2^ + 0.4126P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.377 _refine_diff_density_min -0.225 _refine_ls_extinction_method SHELXL93 _refine_ls_extinction_coef 0.0035(8) 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 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(43) _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 C1A 1 0.6580(3) 0.5956(6) 0.3154(4) 0.0468(11) O1A 1 0.5701(2) 0.5368(4) 0.2543(3) 0.0550(9) C13A 1 0.4985(4) 0.6395(9) 0.2558(7) 0.084(2) H13A 1 0.5056(19) 0.6517(48) 0.3397(9) 0.101 H13B 1 0.4403(5) 0.5877(31) 0.2063(36) 0.101 H13C 1 0.5010(20) 0.7489(21) 0.2223(39) 0.101 C2A 1 0.6822(4) 0.7402(6) 0.3886(5) 0.0543(12) H2A 1 0.6367(4) 0.8121(6) 0.3895(5) 0.065 C3A 1 0.7726(4) 0.7772(7) 0.4592(5) 0.0620(14) H3A 1 0.7878(4) 0.8768(7) 0.5052(5) 0.074 C4A 1 0.8421(4) 0.6702(7) 0.4640(5) 0.0616(14) H4A 1 0.9031(4) 0.6951(7) 0.5158(5) 0.074 C4aA 1 0.8198(4) 0.5230(6) 0.3897(5) 0.0517(12) C5A 1 0.8889(3) 0.3933(7) 0.3998(5) 0.0599(13) H5A 1 0.9449(3) 0.4120(7) 0.4745(5) 0.072 H5B 1 0.9034(3) 0.4002(7) 0.3286(5) 0.072 C6A 1 0.8494(3) 0.2194(7) 0.4046(5) 0.0560(12) H6A 1 0.8947(3) 0.1325(7) 0.4151(5) 0.067 H6B 1 0.8336(3) 0.2136(7) 0.4746(5) 0.067 C6aA 1 0.7651(3) 0.1909(6) 0.2852(4) 0.0466(11) C7A 1 0.7446(4) 0.0411(6) 0.2233(5) 0.0507(12) H7A 1 0.7801(4) -0.0542(6) 0.2583(5) 0.061 C7aA 1 0.6687(4) 0.0303(6) 0.1048(5) 0.0479(11) C8A 1 0.6398(4) -0.1225(7) 0.0380(5) 0.0555(12) H8A 1 0.6675(4) -0.2237(7) 0.0748(5) 0.067 C9A 1 0.5720(4) -0.1233(7) -0.0792(6) 0.0620(14) H9A 1 0.5543(4) -0.2248(7) -0.1225(6) 0.074 C10A 1 0.5284(4) 0.0267(7) -0.1356(5) 0.0589(13) H10A 1 0.4828(4) 0.0244(7) -0.2166(5) 0.071 C11A 1 0.5522(4) 0.1779(6) -0.0727(4) 0.0513(12) H11A 1 0.5230(4) 0.2778(6) -0.1103(4) 0.062 C11aA 1 0.6211(3) 0.1786(5) 0.0491(5) 0.0439(10) N12A 1 0.6447(3) 0.3334(5) 0.1155(4) 0.0441(9) O12A 1 0.6051(2) 0.4721(4) 0.0580(3) 0.0519(8) C12aA 1 0.7092(3) 0.3355(6) 0.2351(4) 0.0428(10) C12bA 1 0.7266(3) 0.4920(5) 0.3083(4) 0.0422(10) C1B 1 0.0953(3) -0.0975(6) 0.0013(5) 0.0483(11) O1B 1 0.0213(3) -0.0370(4) -0.0983(3) 0.0556(9) C13B 1 -0.0130(5) -0.1365(9) -0.2081(6) 0.080(2) H13D 1 -0.0674(18) -0.0846(30) -0.2694(16) 0.096 H13E 1 -0.0275(28) -0.2478(19) -0.1895(11) 0.096 H13F 1 0.0327(12) -0.1443(47) -0.2397(23) 0.096 C2B 1 0.1425(4) -0.2431(6) -0.0004(6) 0.0585(13) H2B 1 0.1194(4) -0.3140(6) -0.0693(6) 0.070 C3B 1 0.2236(4) -0.2834(7) 0.0999(6) 0.0651(15) H3B 1 0.2529(4) -0.3849(7) 0.0999(6) 0.078 C4B 1 0.2620(4) -0.1758(7) 0.2001(6) 0.0636(15) H4B 1 0.3192(4) -0.2006(7) 0.2637(6) 0.076 C4aB 1 0.2152(3) -0.0288(7) 0.2065(5) 0.0544(12) C5B 1 0.2574(4) 0.1002(8) 0.3072(5) 0.0612(13) H5C 1 0.3231(4) 0.0814(8) 0.3510(5) 0.073 H5D 1 0.2308(4) 0.0918(8) 0.3665(5) 0.073 C6B 1 0.2384(3) 0.2748(7) 0.2463(5) 0.0573(13) H6C 1 0.2664(3) 0.3613(7) 0.3090(5) 0.069 H6D 1 0.2649(3) 0.2823(7) 0.1868(5) 0.069 C6aB 1 0.1364(3) 0.3025(6) 0.1814(4) 0.0446(10) C7B 1 0.0956(4) 0.4540(6) 0.1841(5) 0.0504(12) H7B 1 0.1312(4) 0.5482(6) 0.2217(5) 0.061 C7aB 1 -0.0014(4) 0.4647(6) 0.1292(5) 0.0461(11) C8B 1 -0.0482(4) 0.6187(7) 0.1221(5) 0.0600(13) H8B 1 -0.0149(4) 0.7185(7) 0.1488(5) 0.072 C9B 1 -0.1408(4) 0.6225(8) 0.0771(5) 0.0636(14) H9B 1 -0.1706(4) 0.7245(8) 0.0737(5) 0.076 C10B 1 -0.1923(4) 0.4731(7) 0.0354(5) 0.0617(15) H10B 1 -0.2559(4) 0.4770(7) 0.0044(5) 0.074 C11B 1 -0.1497(3) 0.3231(7) 0.0399(5) 0.0527(12) H11B 1 -0.1838(3) 0.2240(7) 0.0140(5) 0.063 C11aB 1 -0.0543(3) 0.3191(6) 0.0838(4) 0.0438(11) N12B 1 -0.0098(3) 0.1638(5) 0.0851(3) 0.0414(8) O12B 1 -0.0587(2) 0.0258(4) 0.0532(3) 0.0515(8) C12aB 1 0.0826(3) 0.1610(5) 0.1212(4) 0.0419(10) C12bB 1 0.1286(3) 0.0052(6) 0.1089(5) 0.0455(11) 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 C1A 0.054(3) 0.002(2) 0.029(2) 0.042(2) 0.009(2) 0.051(2) O1A 0.050(2) 0.0065(15) 0.029(2) 0.052(2) -0.004(2) 0.067(2) C13A 0.066(4) 0.020(3) 0.034(3) 0.083(4) -0.019(4) 0.103(5) C2A 0.075(3) 0.001(2) 0.037(3) 0.043(3) -0.003(2) 0.054(3) C3A 0.089(4) -0.014(3) 0.037(3) 0.050(3) -0.006(2) 0.054(3) C4A 0.072(3) -0.021(3) 0.027(3) 0.070(4) -0.004(2) 0.046(3) C4aA 0.053(3) -0.009(2) 0.028(2) 0.058(3) -0.003(2) 0.050(3) C5A 0.045(3) -0.001(3) 0.022(2) 0.078(4) 0.000(3) 0.056(3) C6A 0.048(3) 0.007(2) 0.016(2) 0.069(3) 0.008(2) 0.047(3) C6aA 0.055(3) 0.001(2) 0.031(2) 0.042(3) -0.001(2) 0.052(3) C7A 0.058(3) 0.012(2) 0.033(2) 0.048(3) 0.010(2) 0.056(3) C7aA 0.054(3) 0.001(2) 0.036(2) 0.043(3) -0.001(2) 0.058(3) C8A 0.067(3) 0.004(2) 0.047(3) 0.043(3) -0.002(2) 0.074(3) C9A 0.070(3) -0.016(3) 0.046(3) 0.052(3) -0.021(3) 0.079(4) C10A 0.060(3) -0.009(3) 0.029(3) 0.071(4) -0.012(3) 0.051(3) C11A 0.062(3) -0.005(2) 0.026(2) 0.047(3) -0.001(2) 0.048(3) C11aA 0.047(2) -0.002(2) 0.026(2) 0.041(2) 0.000(2) 0.049(3) N12A 0.048(2) 0.002(2) 0.021(2) 0.038(2) 0.001(2) 0.047(2) O12A 0.057(2) 0.0093(15) 0.023(2) 0.043(2) 0.0073(15) 0.054(2) C12aA 0.043(2) 0.002(2) 0.021(2) 0.044(3) 0.000(2) 0.044(3) C12bA 0.050(3) -0.001(2) 0.024(2) 0.036(2) 0.001(2) 0.044(3) C1B 0.057(3) -0.003(2) 0.033(2) 0.041(2) 0.002(2) 0.056(3) O1B 0.065(2) 0.001(2) 0.021(2) 0.052(2) -0.0073(15) 0.047(2) C13B 0.079(4) -0.004(3) 0.024(3) 0.080(4) -0.025(3) 0.074(4) C2B 0.074(3) 0.001(3) 0.046(3) 0.043(3) -0.001(2) 0.074(4) C3B 0.078(4) 0.014(3) 0.052(3) 0.056(3) 0.011(3) 0.080(4) C4B 0.056(3) 0.017(3) 0.038(3) 0.071(4) 0.021(3) 0.074(4) C4aB 0.051(3) 0.009(2) 0.030(2) 0.064(3) 0.010(2) 0.056(3) C5B 0.048(3) 0.006(3) 0.018(2) 0.087(4) -0.001(3) 0.047(3) C6B 0.050(3) -0.004(2) 0.020(2) 0.069(3) -0.016(2) 0.051(3) C6aB 0.051(3) -0.002(2) 0.023(2) 0.044(3) -0.006(2) 0.042(2) C7B 0.058(3) -0.009(2) 0.027(2) 0.048(3) -0.007(2) 0.050(3) C7aB 0.059(3) 0.000(2) 0.029(2) 0.045(2) -0.005(2) 0.042(2) C8B 0.081(4) 0.003(3) 0.038(3) 0.045(3) 0.000(2) 0.062(3) C9B 0.082(4) 0.020(3) 0.037(3) 0.058(3) 0.009(3) 0.058(3) C10B 0.057(3) 0.026(3) 0.035(3) 0.078(4) 0.025(3) 0.060(3) C11B 0.049(3) 0.003(2) 0.026(2) 0.065(3) 0.016(2) 0.050(3) C11aB 0.051(3) 0.000(2) 0.023(2) 0.047(3) 0.007(2) 0.039(2) N12B 0.046(2) -0.001(2) 0.018(2) 0.040(2) 0.001(2) 0.038(2) O12B 0.050(2) -0.0092(14) 0.023(2) 0.043(2) -0.0040(15) 0.061(2) C12aB 0.046(2) 0.002(2) 0.020(2) 0.042(2) -0.001(2) 0.039(2) C12bB 0.054(3) 0.003(2) 0.034(2) 0.042(2) 0.004(2) 0.053(3) _cod_database_code 2003270