#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/1/1101008.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_1101008 _journal_name_full 'Journal of Molecular Structure' loop_ _publ_author_name 'Masao Hashimoto' 'Fukue Tajima' 'Kazuo Eda' 'Kimiaki Yamamura' 'Tadashi Okazaki' _chemical_name_common 'n-dodecylurea' _chemical_melting_point 379.2 _chemical_formula_moiety 'C13 H28 N2 O' _chemical_formula_sum 'C13 H28 N2 O' _chemical_formula_weight 228.37 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.430(10) _cell_length_b 7.5982(18) _cell_length_c 9.295(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.624(4) _cell_angle_gamma 90.00 _cell_volume 2982.3(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1003 _cell_measurement_theta_min 2.202 _cell_measurement_theta_max 22.578 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7754 _exptl_absorpt_correction_T_max 0.9974 _exptl_absorpt_process_details 'program SADABS ver. 2.03(Sheldrick)' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7775 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.18 _reflns_number_total 2994 _reflns_number_gt 1392 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2994 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1497 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.19988(6) 0.2601(3) 0.5087(2) 0.0479(6) Uani 1 1 d . . . C2 C 0.18386(6) 0.3999(3) 0.5882(2) 0.0484(6) Uani 1 1 d . . . C3 C 0.17048(6) 0.5466(3) 0.4907(2) 0.0522(6) Uani 1 1 d . . . C4 C 0.15290(6) 0.6861(3) 0.5668(2) 0.0531(6) Uani 1 1 d . . . C5 C 0.13892(7) 0.8298(3) 0.4679(2) 0.0557(6) Uani 1 1 d . . . C6 C 0.12143(7) 0.9695(3) 0.5435(3) 0.0598(7) Uani 1 1 d . . . C7 C 0.10599(7) 1.1093(3) 0.4451(3) 0.0618(7) Uani 1 1 d . . . C8 C 0.08881(7) 1.2503(3) 0.5210(3) 0.0678(7) Uani 1 1 d . . . C9 C 0.07298(8) 1.3882(4) 0.4225(3) 0.0748(8) Uani 1 1 d . . . C10 C 0.05655(8) 1.5323(4) 0.4975(3) 0.0830(9) Uani 1 1 d . . . C11 C 0.04047(11) 1.6672(5) 0.3991(4) 0.1141(12) Uani 1 1 d . . . C12 C 0.02417(8) 1.8093(4) 0.4767(4) 0.1478(15) Uani 1 1 d . . . H12A H 0.0090 1.7570 0.5337 0.222 Uiso 1 1 calc R . . H12B H 0.0136 1.8883 0.4073 0.222 Uiso 1 1 calc R . . H12C H 0.0396 1.8733 0.5387 0.222 Uiso 1 1 calc R . . C1U C 0.22535(4) -0.0257(3) 0.55596(19) 0.0407(5) Uani 1 1 d . . . H1 H 0.2100(4) 0.129(2) 0.692(2) 0.041(6) Uiso 1 1 d . . . H2 H 0.2346(4) -0.120(2) 0.745(2) 0.049(6) Uiso 1 1 d . . . H3 H 0.2459(5) -0.245(3) 0.630(2) 0.081(8) Uiso 1 1 d . . . H1A H 0.1858(4) 0.208(3) 0.433(2) 0.059(6) Uiso 1 1 d . . . H2A H 0.1671(5) 0.353(3) 0.642(2) 0.077(7) Uiso 1 1 d . . . H3A H 0.1564(5) 0.503(3) 0.414(2) 0.081(8) Uiso 1 1 d . . . H4A H 0.1368(5) 0.634(3) 0.624(2) 0.069(7) Uiso 1 1 d . . . H5A H 0.1249(5) 0.780(3) 0.393(3) 0.088(9) Uiso 1 1 d . . . H6A H 0.1050(5) 0.917(3) 0.599(2) 0.078(8) Uiso 1 1 d . . . H7A H 0.0916(5) 1.055(3) 0.372(3) 0.085(8) Uiso 1 1 d . . . H8A H 0.0726(5) 1.194(3) 0.578(2) 0.081(8) Uiso 1 1 d . . . H9A H 0.0576(5) 1.329(3) 0.348(3) 0.090(9) Uiso 1 1 d . . . H10A H 0.0400(7) 1.474(4) 0.550(3) 0.117(11) Uiso 1 1 d . . . H11A H 0.0234(8) 1.582(4) 0.334(4) 0.185(17) Uiso 1 1 d . . . H1B H 0.2183(5) 0.314(3) 0.456(2) 0.065(6) Uiso 1 1 d . . . H2B H 0.1993(4) 0.443(3) 0.668(2) 0.064(6) Uiso 1 1 d . . . H3B H 0.1880(5) 0.593(3) 0.439(2) 0.069(7) Uiso 1 1 d . . . H4B H 0.1682(4) 0.740(3) 0.646(2) 0.067(7) Uiso 1 1 d . . . H5B H 0.1562(5) 0.881(3) 0.413(2) 0.070(7) Uiso 1 1 d . . . H6B H 0.1366(5) 1.023(3) 0.618(2) 0.077(8) Uiso 1 1 d . . . H7B H 0.1228(5) 1.169(3) 0.391(2) 0.063(7) Uiso 1 1 d . . . H8B H 0.1033(6) 1.311(3) 0.596(3) 0.103(10) Uiso 1 1 d . . . H9B H 0.0884(6) 1.435(3) 0.362(3) 0.106(10) Uiso 1 1 d . . . H10B H 0.0726(7) 1.599(4) 0.562(3) 0.117(11) Uiso 1 1 d . . . H11B H 0.0560(8) 1.718(5) 0.339(4) 0.167(18) Uiso 1 1 d . . . N1 N 0.21177(4) 0.1197(2) 0.60348(18) 0.0488(5) Uani 1 1 d . . . N2 N 0.23608(5) -0.1424(3) 0.65656(18) 0.0550(5) Uani 1 1 d . . . O1 O 0.22809(3) -0.04813(17) 0.42583(13) 0.0522(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0679(16) 0.0440(14) 0.0322(11) 0.0025(10) 0.0076(12) 0.0106(12) C2 0.0636(15) 0.0460(15) 0.0362(12) -0.0013(10) 0.0076(12) 0.0092(12) C3 0.0695(16) 0.0452(14) 0.0421(12) 0.0003(11) 0.0073(12) 0.0122(13) C4 0.0689(16) 0.0453(14) 0.0452(13) 0.0015(11) 0.0061(13) 0.0114(13) C5 0.0737(17) 0.0474(15) 0.0462(13) 0.0006(12) 0.0076(13) 0.0139(13) C6 0.0765(17) 0.0521(16) 0.0508(14) -0.0009(13) 0.0064(14) 0.0164(14) C7 0.0749(17) 0.0535(16) 0.0575(15) 0.0043(13) 0.0092(14) 0.0161(14) C8 0.085(2) 0.0568(17) 0.0630(17) 0.0017(13) 0.0130(17) 0.0215(15) C9 0.086(2) 0.0659(19) 0.0724(18) 0.0007(15) 0.0049(18) 0.0263(16) C10 0.089(2) 0.0662(19) 0.094(2) -0.0027(18) 0.011(2) 0.0237(19) C11 0.122(3) 0.089(3) 0.131(3) -0.003(2) 0.007(3) 0.050(3) C12 0.139(3) 0.095(3) 0.209(4) -0.018(3) 0.015(3) 0.060(2) C1U 0.0539(12) 0.0365(13) 0.0319(11) -0.0012(9) 0.0052(9) 0.0051(10) N1 0.0736(12) 0.0463(11) 0.0269(10) -0.0010(8) 0.0063(9) 0.0141(10) N2 0.0893(14) 0.0504(12) 0.0261(10) 0.0018(9) 0.0100(10) 0.0195(11) O1 0.0857(11) 0.0454(9) 0.0267(7) 0.0004(6) 0.0114(6) 0.0135(8)