#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/50/2005068.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2005068 loop_ _publ_author_name 'Kowalski, A.' _publ_section_title ; 1-(p-Methoxyphenyl)-2-methyl-4-nitroimidazole and 1-(p-Acetylphenyl)-2-methyl-4-nitroimidazole ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1784 _journal_page_last 1787 _journal_paper_doi 10.1107/S0108270196001722 _journal_volume 52 _journal_year 1996 _chemical_formula_sum 'C12 H11 N3 O3' _chemical_formula_weight 245.24 _chemical_name_systematic ; 1-(p-acetyl-phenyl)-2-methyl-4-nitro-imidazole ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL _cell_angle_alpha 90.46(2) _cell_angle_beta 105.24(2) _cell_angle_gamma 110.59(2) _cell_formula_units_Z 2 _cell_length_a 7.4930(10) _cell_length_b 8.217(2) _cell_length_c 10.332(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 32 _cell_measurement_theta_min 16 _cell_volume 571.0(2) _computing_data_collection 'Kuma KM-4 User's Guide (Kuma, 1989)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Kuma KM-4 automated four-circle \k-axis' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0105 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2517 _diffrn_reflns_theta_max 81.53 _diffrn_reflns_theta_min 4.46 _diffrn_standards_decay_% 4 _diffrn_standards_interval_count 50 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.882 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_meas 1.4 _exptl_crystal_density_method flotation _exptl_crystal_description irregular _exptl_crystal_F_000 256 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _refine_diff_density_max 0.108 _refine_diff_density_min -0.115 _refine_ls_extinction_coef 0.022(4) _refine_ls_extinction_method SHELXL93 _refine_ls_goodness_of_fit_all 0.855 _refine_ls_goodness_of_fit_obs 0.738 _refine_ls_hydrogen_treatment 'H atoms refined as rigid groups' _refine_ls_matrix_type full _refine_ls_number_parameters 171 _refine_ls_number_reflns 1606 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.392 _refine_ls_restrained_S_obs 0.738 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_obs 0.0424 _refine_ls_shift/esd_max 0.013 _refine_ls_shift/esd_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.1134P)^2^ + 0.4209P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_wR_factor_all 0.2912 _refine_ls_wR_factor_obs 0.1147 _reflns_number_observed 1282 _reflns_number_total 2344 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file ab1279.cif _[local]_cod_data_source_block II _cod_database_code 2005068 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0651(12) 0.0661(13) 0.0597(12) 0.0367(10) 0.0205(10) 0.0046(9) O2 0.089(2) 0.0654(14) 0.0704(14) 0.0393(12) 0.0343(12) 0.0301(11) O4 0.0750(14) 0.0535(13) 0.0658(13) 0.0271(11) 0.0187(10) 0.0167(10) N1 0.0473(12) 0.0464(12) 0.0375(11) 0.0199(10) 0.0129(9) 0.0064(9) N2 0.0501(12) 0.0554(14) 0.0388(11) 0.0231(10) 0.0127(9) 0.0080(10) N3 0.0562(13) 0.0464(13) 0.0436(12) 0.0222(11) 0.0121(10) 0.0020(10) C1 0.0448(14) 0.052(2) 0.0352(12) 0.0184(12) 0.0106(10) 0.0061(11) C2 0.0477(14) 0.0428(14) 0.0363(13) 0.0193(11) 0.0111(10) 0.0022(10) C3 0.0475(14) 0.051(2) 0.0429(14) 0.0207(12) 0.0157(11) 0.0049(11) C4 0.0412(13) 0.0442(14) 0.0404(13) 0.0154(11) 0.0121(10) 0.0072(11) C5 0.062(2) 0.052(2) 0.0395(14) 0.0230(13) 0.0104(12) 0.0021(12) C6 0.058(2) 0.044(2) 0.0479(15) 0.0194(12) 0.0126(12) 0.0031(12) C7 0.0390(13) 0.050(2) 0.0439(14) 0.0174(11) 0.0128(10) 0.0098(11) C8 0.057(2) 0.051(2) 0.0390(14) 0.0220(13) 0.0152(11) 0.0062(11) C9 0.056(2) 0.0430(15) 0.0444(14) 0.0205(12) 0.0158(11) 0.0037(11) C10 0.063(2) 0.080(2) 0.052(2) 0.041(2) 0.0221(13) 0.0184(14) C12 0.0421(14) 0.055(2) 0.055(2) 0.0207(12) 0.0164(11) 0.0146(13) C13 0.072(2) 0.076(2) 0.054(2) 0.037(2) 0.0237(14) 0.0234(15) 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 _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol O1 1 0.5960(3) -0.2303(3) 0.3401(2) 0.0595(6) Uani d . O O2 1 0.4104(3) -0.3140(3) 0.4735(2) 0.0694(7) Uani d . O O4 1 0.2533(3) 0.7331(3) -0.1047(2) 0.0640(6) Uani d . O N1 1 0.2862(3) 0.0915(3) 0.2284(2) 0.0428(6) Uani d . N N2 1 0.2342(3) -0.0779(3) 0.3919(2) 0.0470(6) Uani d . N N3 1 0.4643(3) -0.2233(3) 0.3873(2) 0.0482(6) Uani d . N C1 1 0.1851(4) 0.0425(3) 0.3250(2) 0.0439(6) Uani d . C C2 1 0.3699(3) -0.1032(3) 0.3379(2) 0.0417(6) Uani d . C C3 1 0.4055(4) -0.0039(3) 0.2371(2) 0.0457(7) Uani d . C H3 1 0.4939(27) -0.0010(3) 0.1839(16) 0.055 Uiso calc R H C4 1 0.2670(3) 0.2144(3) 0.1324(2) 0.0419(6) Uani d . C C5 1 0.2885(4) 0.3811(3) 0.1769(3) 0.0512(7) Uani d . C H5 1 0.3170(10) 0.4158(12) 0.2719(32) 0.061 Uiso calc R H C6 1 0.2687(4) 0.4975(4) 0.0835(3) 0.0503(7) Uani d . C H6 1 0.2826(6) 0.6177(38) 0.1145(10) 0.060 Uiso calc R H C7 1 0.2299(3) 0.4494(3) -0.0527(2) 0.0436(6) Uani d . C C8 1 0.2114(4) 0.2816(3) -0.0949(3) 0.0480(7) Uani d . C H8 1 0.1857(9) 0.2471(11) -0.1898(30) 0.058 Uiso calc R H C9 1 0.2294(4) 0.1635(4) -0.0023(3) 0.0470(7) Uani d . C H9 1 0.2163(6) 0.0517(37) -0.0306(10) 0.056 Uiso calc R H C10 1 0.0423(4) 0.1177(4) 0.3480(3) 0.0593(8) Uani d . C H10A 1 -0.0239(14) 0.1464(7) 0.2653(16) 0.089 Uiso calc R H H10B 1 0.1112(13) 0.2198(20) 0.4100(12) 0.089 Uiso calc R H H10C 1 -0.0518(19) 0.0350(16) 0.3833(7) 0.089 Uiso calc R H C12 1 0.2179(4) 0.5830(4) -0.1489(3) 0.0491(7) Uani d . C C13 1 0.1649(5) 0.5318(4) -0.2971(3) 0.0630(8) Uani d . C H13A 1 0.0276(27) 0.4466(17) -0.3284(7) 0.095 Uiso calc R H H13B 1 0.2562(18) 0.4789(11) -0.3154(5) 0.095 Uiso calc R H H13C 1 0.1760(5) 0.6362(20) -0.3452(10) 0.095 Uiso calc R H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C3 N1 C1 107.3(2) n C3 N1 C4 125.3(2) n C1 N1 C4 127.3(2) n C1 N2 C2 104.3(2) n O1 N3 O2 123.2(2) n O2 N3 C2 119.0(2) n O1 N3 C2 117.8(2) n N2 C1 N1 110.9(2) n N2 C1 C10 125.4(2) n N1 C1 C10 123.7(2) n N2 C2 C3 113.5(2) n N2 C2 N3 121.4(2) n C3 C2 N3 125.1(2) n C2 C3 N1 103.9(2) n C5 C4 C9 121.3(2) n C5 C4 N1 119.7(2) n C9 C4 N1 119.0(2) n C6 C5 C4 119.0(2) n C5 C6 C7 120.8(2) n C6 C7 C12 118.5(2) n C8 C7 C12 122.3(2) n C8 C7 C6 119.1(2) n C7 C8 C9 120.5(2) n C4 C9 C8 119.2(2) n O4 C12 C13 120.9(2) n O4 C12 C7 119.4(2) n C13 C12 C7 119.6(2) n C2 C3 H3 128.02(15) n N1 C3 H3 128.03(13) n C6 C5 H5 120.5(2) n C4 C5 H5 120.51(15) n C5 C6 H6 119.6(2) n C7 C6 H6 119.6(2) n C9 C8 H8 119.7(2) n C7 C8 H8 119.74(14) n C4 C9 H9 120.4(2) n C8 C9 H9 120.4(2) n C1 C10 H10A 109.47(14) n C1 C10 H10B 109.5(2) n H10A C10 H10B 109.5 n C1 C10 H10C 109.5(2) n H10A C10 H10C 109.5 n H10B C10 H10C 109.5 n C12 C13 H13A 109.5(2) n C12 C13 H13B 109.47(15) n H13A C13 H13B 109.5 n C12 C13 H13C 109.5(2) n H13A C13 H13C 109.5 n H13B C13 H13C 109.5 n loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 N3 1.228(3) yes O2 N3 1.225(3) yes O4 C12 1.224(3) yes N1 C3 1.368(3) yes N1 C1 1.386(3) yes N1 C4 1.437(3) yes N2 C1 1.314(3) yes N2 C2 1.354(3) yes N3 C2 1.430(3) yes C1 C10 1.476(4) yes C2 C3 1.352(3) yes C4 C5 1.382(3) yes C4 C9 1.376(3) yes C5 C6 1.381(4) yes C6 C7 1.384(4) yes C7 C8 1.390(4) yes C7 C12 1.497(4) yes C8 C9 1.384(4) yes C12 C13 1.494(4) yes C3 H3 0.96(3) n C5 H5 0.97(3) n C6 H6 1.00(3) n C8 H8 0.97(3) n C9 H9 0.92(3) n C10 H10A 0.95(2) n C10 H10B 0.95(2) n C10 H10C 0.95(2) n C13 H13A 0.98(2) n C13 H13B 0.98(2) n C13 H13C 0.98(2) n