#------------------------------------------------------------------------------ #$Date: 2016-02-13 12:50:18 +0000 (Sat, 13 Feb 2016) $ #$Revision: 176428 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/10/1101009.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_1101009 loop_ _publ_author_name 'Hashimoto, Masao' 'Tajima, Fukue' 'Eda, Kazuo' 'Yamamura, Kimiaki' 'Okazaki, Tadashi' _publ_section_title ; Exploration of plastic-like phases in alkylurea systems. A thermal and X-ray study ; _journal_issue 1-3 _journal_name_full 'Journal of Molecular Structure' _journal_page_first 23 _journal_page_last 33 _journal_paper_doi 10.1016/j.molstruc.2004.08.008 _journal_volume 734 _journal_year 2005 _chemical_formula_moiety 'C13 H28 N2 O' _chemical_formula_sum 'C13 H28 N2 O' _chemical_formula_weight 228.37 _chemical_melting_point 379.2 _chemical_name_common n-dodecylurea _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 95.085(8) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 21.100(9) _cell_length_b 7.364(3) _cell_length_c 9.200(4) _cell_measurement_reflns_used 963 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 23.842 _cell_measurement_theta_min 2.908 _cell_volume 1423.8(10) _diffrn_ambient_temperature 293(2) _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.1499 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 7411 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_min 2.91 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_T_max 0.9973 _exptl_absorpt_correction_T_min 0.4957 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'program SADABS ver. 2.03(Sheldrick)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.065 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.04 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.845 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 257 _refine_ls_number_reflns 2916 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.845 _refine_ls_R_factor_all 0.1762 _refine_ls_R_factor_gt 0.0793 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1205P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1874 _refine_ls_wR_factor_ref 0.2223 _reflns_number_gt 1331 _reflns_number_total 2916 _reflns_threshold_expression >2sigma(I) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1101009 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 0.10187(18) 0.9789(4) 0.0541(3) 0.0308(8) Uani 1 1 d . . . C2 C 0.13209(18) 0.8335(4) 0.1506(3) 0.0316(8) Uani 1 1 d . . . C3 C 0.16067(17) 0.6833(4) 0.0669(3) 0.0336(8) Uani 1 1 d . . . C4 C 0.19353(18) 0.5397(4) 0.1614(3) 0.0331(8) Uani 1 1 d . . . C5 C 0.22440(18) 0.3926(4) 0.0768(3) 0.0362(8) Uani 1 1 d . . . C6 C 0.25611(18) 0.2480(4) 0.1727(3) 0.0382(8) Uani 1 1 d . . . C7 C 0.28963(19) 0.1022(5) 0.0912(4) 0.0405(8) Uani 1 1 d . . . C8 C 0.32053(19) -0.0436(4) 0.1884(4) 0.0424(9) Uani 1 1 d . . . C9 C 0.3548(2) -0.1858(5) 0.1084(4) 0.0465(9) Uani 1 1 d . . . C10 C 0.3837(2) -0.3352(5) 0.2058(4) 0.0489(10) Uani 1 1 d . . . C11 C 0.4193(3) -0.4768(6) 0.1257(5) 0.0700(13) Uani 1 1 d . . . C12 C 0.4480(3) -0.6216(8) 0.2247(9) 0.100(2) Uani 1 1 d . . . C1U C 0.04963(14) 1.2710(4) 0.0795(3) 0.0271(7) Uani 1 1 d . . . H1 H 0.0780(14) 1.117(4) 0.242(3) 0.043(9) Uiso 1 1 d . . . H2 H 0.0300(15) 1.370(5) 0.257(4) 0.052(10) Uiso 1 1 d . . . H3 H 0.0055(14) 1.497(4) 0.132(3) 0.035(8) Uiso 1 1 d . . . H1A H 0.1341(15) 1.025(4) 0.000(3) 0.047(10) Uiso 1 1 d . . . H2A H 0.1669(16) 0.885(5) 0.213(4) 0.057(11) Uiso 1 1 d . . . H3A H 0.1953(15) 0.733(4) 0.008(3) 0.050(10) Uiso 1 1 d . . . H4A H 0.2296(14) 0.593(4) 0.228(3) 0.034(8) Uiso 1 1 d . . . H5A H 0.2563(14) 0.452(4) 0.017(3) 0.039(9) Uiso 1 1 d . . . H6A H 0.2886(15) 0.301(5) 0.243(3) 0.047(9) Uiso 1 1 d . . . H7A H 0.3226(15) 0.158(4) 0.034(3) 0.047(10) Uiso 1 1 d . . . H8A H 0.3527(18) 0.018(5) 0.270(4) 0.071(12) Uiso 1 1 d . . . H9A H 0.3894(15) -0.132(4) 0.063(3) 0.042(9) Uiso 1 1 d . . . H10A H 0.4150(17) -0.277(5) 0.275(4) 0.058(11) Uiso 1 1 d . . . H11A H 0.457(2) -0.414(6) 0.074(4) 0.085(14) Uiso 1 1 d . . . H12A H 0.486(3) -0.582(8) 0.298(6) 0.13(2) Uiso 1 1 d . . . H1B H 0.0638(14) 0.932(4) -0.009(3) 0.039(9) Uiso 1 1 d . . . H2B H 0.0980(15) 0.791(5) 0.208(4) 0.051(10) Uiso 1 1 d . . . H3B H 0.1262(15) 0.631(4) 0.004(3) 0.045(9) Uiso 1 1 d . . . H4B H 0.1611(18) 0.480(5) 0.218(4) 0.076(13) Uiso 1 1 d . . . H5B H 0.1901(15) 0.336(4) 0.008(3) 0.046(9) Uiso 1 1 d . . . H6B H 0.2218(16) 0.194(5) 0.224(3) 0.050(10) Uiso 1 1 d . . . H7B H 0.2556(15) 0.041(4) 0.022(3) 0.044(9) Uiso 1 1 d . . . H8B H 0.2849(17) -0.097(5) 0.243(4) 0.059(11) Uiso 1 1 d . . . H9B H 0.3189(17) -0.242(5) 0.037(4) 0.067(12) Uiso 1 1 d . . . H10B H 0.3437(17) -0.393(5) 0.247(4) 0.065(11) Uiso 1 1 d . . . H11B H 0.386(2) -0.541(7) 0.061(5) 0.103(17) Uiso 1 1 d . . . H12B H 0.469(2) -0.715(7) 0.179(5) 0.103(17) Uiso 1 1 d . . . H12C H 0.415(3) -0.677(8) 0.274(6) 0.13(2) Uiso 1 1 d . . . N1 N 0.07706(13) 1.1226(3) 0.1395(2) 0.0315(7) Uani 1 1 d . . . N2 N 0.02830(14) 1.3927(4) 0.1692(3) 0.0353(7) Uani 1 1 d . . . O1 O 0.04504(10) 1.2944(3) -0.05517(18) 0.0348(6) 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 0.051(2) 0.0218(16) 0.0204(14) 0.0015(12) 0.0064(14) 0.0056(15) C2 0.051(2) 0.0224(17) 0.0217(14) 0.0026(12) 0.0059(14) 0.0040(14) C3 0.053(2) 0.0219(17) 0.0262(15) 0.0017(13) 0.0065(15) 0.0029(15) C4 0.051(2) 0.0217(17) 0.0268(15) 0.0006(13) 0.0044(15) 0.0020(15) C5 0.055(2) 0.0228(17) 0.0317(16) -0.0003(14) 0.0075(15) 0.0045(16) C6 0.058(2) 0.0222(18) 0.0349(17) 0.0023(14) 0.0046(16) 0.0030(16) C7 0.056(2) 0.0254(18) 0.0401(18) -0.0001(15) 0.0061(17) 0.0035(16) C8 0.060(3) 0.0248(19) 0.0430(18) 0.0024(16) 0.0078(18) 0.0088(17) C9 0.059(3) 0.032(2) 0.050(2) 0.0029(17) 0.0110(19) 0.0110(17) C10 0.054(3) 0.029(2) 0.064(2) 0.0024(17) 0.005(2) 0.0058(17) C11 0.069(3) 0.038(2) 0.103(4) -0.002(2) 0.008(3) 0.019(2) C12 0.077(4) 0.048(3) 0.172(6) 0.010(4) -0.003(4) 0.026(3) C1U 0.0445(19) 0.0175(15) 0.0195(14) 0.0013(11) 0.0048(12) -0.0021(13) N1 0.0634(18) 0.0161(13) 0.0158(12) 0.0023(10) 0.0080(11) 0.0105(12) N2 0.072(2) 0.0234(15) 0.0119(12) 0.0015(11) 0.0088(11) 0.0161(13) O1 0.0750(16) 0.0192(11) 0.0106(9) 0.0022(8) 0.0058(9) 0.0060(10)