#------------------------------------------------------------------------------ #$Date: 2016-02-13 12:50:18 +0000 (Sat, 13 Feb 2016) $ #$Revision: 176428 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/10/1101011.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_1101011 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 'C14 H30 N2 O' _chemical_formula_sum 'C14 H30 N2 O' _chemical_formula_weight 242.40 _chemical_melting_point 384.6 _chemical_name_common n-tridecylurea _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 99.290(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 22.936(5) _cell_length_b 7.4127(16) _cell_length_c 9.314(2) _cell_measurement_reflns_used 1675 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 23.804 _cell_measurement_theta_min 2.216 _cell_volume 1562.8(6) _diffrn_ambient_temperature 298(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 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 8569 _diffrn_reflns_theta_max 27.55 _diffrn_reflns_theta_min 1.80 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_correction_T_min 0.156955 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'program SADABS ver. 2.03(Sheldrick)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.030 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.58 _exptl_crystal_size_min 0.09 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 274 _refine_ls_number_reflns 3232 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.883 _refine_ls_R_factor_all 0.1381 _refine_ls_R_factor_gt 0.0729 _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^)+(0.0965P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1601 _refine_ls_wR_factor_ref 0.1827 _reflns_number_gt 1552 _reflns_number_total 3232 _reflns_threshold_expression >2sigma(I) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1101011 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 C1U C 0.04695(9) -0.2701(3) -0.0505(2) 0.0404(6) Uani 1 1 d . . . N1 N 0.07239(9) -0.1231(3) -0.0937(2) 0.0463(5) Uani 1 1 d . . . N2 N 0.02635(10) -0.3918(3) -0.1514(2) 0.0545(6) Uani 1 1 d . . . O1 O 0.04271(7) -0.2939(2) 0.08057(14) 0.0526(5) Uani 1 1 d . . . C4 C 0.18294(12) 0.4563(3) -0.0510(2) 0.0494(6) Uani 1 1 d . . . C3 C 0.15193(12) 0.3141(3) 0.0249(2) 0.0485(6) Uani 1 1 d . . . C1 C 0.09631(12) 0.0201(3) 0.0043(2) 0.0459(6) Uani 1 1 d . . . C7 C 0.27368(13) 0.8921(4) 0.0695(3) 0.0562(7) Uani 1 1 d . . . C5 C 0.21227(13) 0.6039(4) 0.0491(3) 0.0510(6) Uani 1 1 d . . . C6 C 0.24232(13) 0.7464(4) -0.0280(3) 0.0549(7) Uani 1 1 d . . . C2 C 0.12478(12) 0.1646(3) -0.0742(2) 0.0466(6) Uani 1 1 d . . . C8 C 0.30250(13) 1.0351(4) -0.0108(3) 0.0577(7) Uani 1 1 d . . . C9 C 0.33524(14) 1.1789(4) 0.0869(3) 0.0627(7) Uani 1 1 d . . . C10 C 0.36346(15) 1.3227(4) 0.0056(3) 0.0661(8) Uani 1 1 d . . . C11 C 0.39683(17) 1.4675(4) 0.1007(4) 0.0761(9) Uani 1 1 d . . . C12 C 0.42205(18) 1.6129(5) 0.0165(5) 0.0899(11) Uani 1 1 d . . . C13 C 0.4573(3) 1.7526(7) 0.1122(9) 0.1325(19) Uani 1 1 d . . . H3B H 0.1201(8) 0.372(3) 0.067(2) 0.040(6) Uiso 1 1 d . . . H3A H 0.1797(9) 0.266(3) 0.103(2) 0.054(7) Uiso 1 1 d . . . H6A H 0.2727(10) 0.680(3) -0.082(3) 0.066(7) Uiso 1 1 d . . . H5B H 0.1809(9) 0.665(3) 0.095(2) 0.056(7) Uiso 1 1 d . . . H7A H 0.3037(10) 0.835(3) 0.147(3) 0.065(7) Uiso 1 1 d . . . H10B H 0.3327(12) 1.384(4) -0.063(3) 0.089(10) Uiso 1 1 d . . . H8A H 0.3308(10) 0.975(3) -0.063(3) 0.058(7) Uiso 1 1 d . . . H1A H 0.1268(9) -0.032(3) 0.081(2) 0.055(7) Uiso 1 1 d . . . H4A H 0.2123(9) 0.394(3) -0.099(2) 0.049(6) Uiso 1 1 d . . . H5A H 0.2420(11) 0.553(4) 0.122(3) 0.075(8) Uiso 1 1 d . . . H9A H 0.3636(13) 1.125(4) 0.163(3) 0.093(10) Uiso 1 1 d . . . H10A H 0.3906(11) 1.258(4) -0.044(3) 0.079(9) Uiso 1 1 d . . . H8B H 0.2697(13) 1.098(4) -0.083(3) 0.096(10) Uiso 1 1 d . . . H1B H 0.0632(10) 0.083(4) 0.053(3) 0.068(7) Uiso 1 1 d . . . H6B H 0.2137(12) 0.800(4) -0.092(3) 0.081(9) Uiso 1 1 d . . . H2A H 0.1550(10) 0.112(3) -0.119(2) 0.054(7) Uiso 1 1 d . . . H7B H 0.2436(10) 0.952(3) 0.122(2) 0.057(7) Uiso 1 1 d . . . H11A H 0.4302(15) 1.421(5) 0.162(4) 0.110(12) Uiso 1 1 d . . . H9B H 0.3050(10) 1.238(4) 0.141(3) 0.075(8) Uiso 1 1 d . . . H12B H 0.3874(18) 1.662(6) -0.058(5) 0.152(17) Uiso 1 1 d . . . H4B H 0.1541(12) 0.515(4) -0.124(3) 0.097(10) Uiso 1 1 d . . . H12A H 0.4480(15) 1.548(5) -0.049(4) 0.127(13) Uiso 1 1 d . . . H2B H 0.0961(12) 0.205(4) -0.148(3) 0.098(10) Uiso 1 1 d . . . H13A H 0.495(2) 1.687(7) 0.169(5) 0.17(2) Uiso 1 1 d . . . H13B H 0.4308(17) 1.828(6) 0.168(4) 0.138(15) Uiso 1 1 d . . . H11B H 0.3695(12) 1.521(4) 0.159(3) 0.082(9) Uiso 1 1 d . . . H2 H 0.0275(9) -0.373(3) -0.234(3) 0.055(7) Uiso 1 1 d . . . H1 H 0.0755(11) -0.103(4) -0.172(3) 0.064(8) Uiso 1 1 d . . . H3 H 0.0022(10) -0.495(4) -0.130(2) 0.061(7) Uiso 1 1 d . . . H13C H 0.4703(18) 1.836(6) 0.059(5) 0.136(17) Uiso 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 C1U 0.0618(14) 0.0356(14) 0.0227(11) 0.0000(9) 0.0032(9) -0.0002(11) N1 0.0760(13) 0.0404(13) 0.0218(10) -0.0009(8) 0.0061(9) -0.0142(10) N2 0.0928(16) 0.0508(14) 0.0195(10) -0.0033(9) 0.0077(9) -0.0213(12) O1 0.0941(12) 0.0429(10) 0.0213(8) -0.0016(7) 0.0111(7) -0.0107(9) C4 0.0686(17) 0.0407(16) 0.0379(13) -0.0007(11) 0.0058(12) -0.0077(13) C3 0.0688(16) 0.0391(15) 0.0365(13) 0.0006(11) 0.0050(12) -0.0035(12) C1 0.0679(16) 0.0403(15) 0.0278(11) -0.0016(10) 0.0023(11) -0.0086(12) C7 0.0752(18) 0.0421(16) 0.0497(14) -0.0030(13) 0.0055(14) -0.0067(14) C5 0.0700(17) 0.0412(16) 0.0398(13) -0.0015(11) 0.0028(12) -0.0058(13) C6 0.0747(18) 0.0430(17) 0.0458(14) -0.0007(12) 0.0063(13) -0.0074(14) C2 0.0674(16) 0.0379(15) 0.0333(12) -0.0008(10) 0.0047(12) -0.0098(12) C8 0.0754(19) 0.0423(17) 0.0556(15) -0.0061(13) 0.0108(14) -0.0123(14) C9 0.082(2) 0.0484(18) 0.0557(16) -0.0037(14) 0.0058(15) -0.0113(15) C10 0.078(2) 0.0509(19) 0.0687(19) -0.0036(15) 0.0092(16) -0.0125(15) C11 0.083(2) 0.057(2) 0.086(2) -0.0081(18) 0.008(2) -0.0133(18) C12 0.092(2) 0.056(2) 0.125(3) -0.008(2) 0.026(2) -0.0245(19) C13 0.126(4) 0.081(4) 0.198(6) -0.033(4) 0.048(4) -0.038(3)