#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/53/2105329.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_2105329 loop_ _publ_author_name 'N\"ather, Christian' 'D\"oring, Cindy' 'Jess, Inke' 'Jones, Peter G.' 'Taouss, Christina' _publ_section_title ; Thermodynamic and structural relationships between the two polymorphs of 1,3-dimethylurea ; _journal_coeditor_code PS5022 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 70 _journal_page_last 76 _journal_volume 69 _journal_year 2013 _chemical_formula_sum 'C3 H8 N2 O' _chemical_formula_weight 88.11 _chemical_name_systematic ; 1,3-dimethylurea ; _space_group_IT_number 18 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2 2ab' _symmetry_space_group_name_H-M 'P 21 21 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 10.8522(6) _cell_length_b 4.9102(3) _cell_length_c 4.5766(3) _cell_measurement_reflns_used 6268 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.6502 _cell_measurement_theta_min 3.7475 _cell_volume 243.87(3) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 16.1419 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0065 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 11695 _diffrn_reflns_theta_full 27.84 _diffrn_reflns_theta_max 27.84 _diffrn_reflns_theta_min 3.76 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.82692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description tablet _exptl_crystal_F_000 96 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.125 _refine_diff_density_min -0.142 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 10(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 371 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.144 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0288 _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^)+(0.0386P)^2^+0.0474P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.0771 _reflns_number_gt 367 _reflns_number_total 371 _reflns_threshold_expression >2sigma(I) _journal_paper_doi 10.1107/S0108768112049324 _iucr_refine_instructions_details ; TITL Bonn in P2(1)2(1)2 REM P2(1)2(1)2 (#18 in standard setting) CELL 0.71073 10.8522 4.9102 4.5766 90.0000 90.0000 90.0000 ZERR 2.00 0.0006 0.0003 0.0003 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z SYMM -x+1/2, y+1/2,-z SYMM x+1/2,-y+1/2,-z SFAC C H N O UNIT 6.00 16.00 4.00 2.00 EQIV $1 x, y, z+1 HTAB N1 O1_$1 ACTA CONF SHEL 999 0.76 TEMP -173 SIZE 0.2 0.5 0.6 MERG 3 L.S. 4 FMAP 2 PLAN 10 WGHT 0.038600 0.047400 FVAR 29.63122 N1 3 0.425117 0.664294 0.873522 11.00000 0.02551 0.02947 = 0.01858 0.00036 0.00039 0.00541 H01 2 0.431973 0.659012 1.067315 11.00000 0.03191 O1 4 0.500000 0.500000 0.445592 10.50000 0.03599 0.03692 = 0.01647 0.00000 0.00000 0.00627 C1 1 0.500000 0.500000 0.716793 10.50000 0.01996 0.02359 = 0.01830 0.00000 0.00000 -0.00209 C2 1 0.343783 0.857333 0.732371 11.00000 0.02373 0.02871 = 0.03084 0.00023 -0.00361 0.00438 AFIX 137 H2A 2 0.390371 0.963429 0.588526 11.00000 -1.50000 H2B 2 0.308803 0.980247 0.879280 11.00000 -1.50000 H2C 2 0.277103 0.759030 0.633735 11.00000 -1.50000 HKLF 4 ; _[local]_cod_data_source_file ps5022.cif _[local]_cod_data_source_block bonn _cod_database_code 2105329 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity N N1 0.42512(9) 0.6643(3) 0.8735(3) 0.0245(3) Uani d . 1 1 H H01 0.4320(14) 0.659(4) 1.067(4) 0.032(4) Uiso d . 1 1 O O1 0.5000 0.5000 0.4456(3) 0.0298(4) Uani d S 1 2 C C1 0.5000 0.5000 0.7168(4) 0.0206(4) Uani d S 1 2 C C2 0.34378(11) 0.8573(3) 0.7324(3) 0.0278(3) Uani d . 1 1 H H2A 0.3904 0.9634 0.5885 0.042 Uiso calc R 1 1 H H2B 0.3088 0.9802 0.8793 0.042 Uiso calc R 1 1 H H2C 0.2771 0.7590 0.6337 0.042 Uiso calc R 1 1 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 N1 0.0255(5) 0.0295(5) 0.0186(5) 0.0054(5) 0.0004(4) 0.0004(5) O1 0.0360(7) 0.0369(8) 0.0165(6) 0.0063(7) 0.000 0.000 C1 0.0200(7) 0.0236(8) 0.0183(7) -0.0021(7) 0.000 0.000 C2 0.0237(5) 0.0287(6) 0.0308(7) 0.0044(5) -0.0036(6) 0.0002(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle C1 N1 C2 . . 121.39(12) O1 C1 N1 . 2_665 122.06(8) O1 C1 N1 . . 122.06(8) N1 C1 N1 2_665 . 115.87(15) C1 N1 H01 . . 117.5(11) C2 N1 H01 . . 121.0(12) N1 C2 H2A . . 109.5 N1 C2 H2B . . 109.5 H2A C2 H2B . . 109.5 N1 C2 H2C . . 109.5 H2A C2 H2C . . 109.5 H2B C2 H2C . . 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance N1 C1 . 1.3512(14) N1 C2 . 1.4474(17) O1 C1 . 1.241(2) C1 N1 2_665 1.3512(14) N1 H01 . 0.890(19) C2 H2A . 0.9800 C2 H2B . 0.9800 C2 H2C . 0.9800 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H01 O1 1_556 0.890(19) 2.038(19) 2.8576(17) 152.6(16) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_4 _geom_torsion C2 N1 C1 O1 . -2.36(13) C2 N1 C1 N1 2_665 177.64(13) _cod_database_fobs_code 2105329