#------------------------------------------------------------------------------ #$Date: 2013-03-09 18:27:54 +0200 (Sat, 09 Mar 2013) $ #$Revision: 75392 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/53/2105328.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_2105328 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 43 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'F 2 -2d' _symmetry_space_group_name_H-M 'F d d 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 8 _cell_length_a 11.3837(2) _cell_length_b 19.6293(4) _cell_length_c 4.56079(13) _cell_measurement_reflns_used 7072 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 75.6880 _cell_measurement_theta_min 4.5014 _cell_volume 1019.13(4) _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 180(2) _diffrn_detector_area_resol_mean 10.3543 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0039 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 8220 _diffrn_reflns_theta_full 75.00 _diffrn_reflns_theta_max 75.88 _diffrn_reflns_theta_min 9.01 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.66812 _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 1.149 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 384 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.078 _refine_diff_density_min -0.116 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.6(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 300 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.123 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0294 _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^)+(0.0529P)^2^+0.1325P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.0804 _reflns_number_gt 299 _reflns_number_total 300 _reflns_threshold_expression >2sigma(I) _journal_paper_doi 10.1107/S0108768112049324 _iucr_refine_instructions_details ; TITL Berlin1 in Fdd2 CELL 1.54184 11.383668 19.629260 4.560794 90.000 90.000 90.000 ZERR 8.00 0.000239 0.000421 0.000128 0.000 0.000 0.000 LATT -4 SYMM -X, -Y, Z SYMM 0.25+X, 0.25-Y, 0.25+Z SYMM 0.25-X, 0.25+Y, 0.25+Z SFAC C H N O UNIT 24 64 16 8 TEMP -93 SIZE 0.15 0.15 0.12 OMIT 3 7 1 ACTA 150 CONF L.S. 4 FMAP 2 EQIV $1 x, y, z+1 HTAB N1 O1_$1 PLAN 10 MERG 3 WGHT 0.052900 0.132500 FVAR 0.28490 C1 1 0.500000 0.500000 0.538811 10.50000 0.05439 0.06276 = 0.03971 0.00000 0.00000 0.00026 N1 3 0.584198 0.468704 0.695186 11.00000 0.05484 0.06834 = 0.04484 0.00143 0.00240 0.00732 H01 2 0.577117 0.469873 0.881088 11.00000 0.05811 C2 1 0.672256 0.426321 0.560913 11.00000 0.06403 0.08454 = 0.07868 0.00028 0.01341 0.01583 AFIX 137 H2A 2 0.634041 0.389172 0.453634 11.00000 -1.50000 H2B 2 0.723427 0.407271 0.713015 11.00000 -1.50000 H2C 2 0.719250 0.453667 0.424674 11.00000 -1.50000 AFIX 0 O1 4 0.500000 0.500000 0.268060 10.50000 0.09299 0.13577 = 0.03850 0.00000 0.00000 0.02947 HKLF 4 ; _[local]_cod_data_source_file ps5022.cif _[local]_cod_data_source_block berlin _cod_original_cell_volume 1019.12(4) _cod_database_code 2105328 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' 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 C C1 0.5000 0.5000 0.5388(5) 0.0523(5) Uani d S 1 2 N N1 0.58420(9) 0.46870(6) 0.6952(3) 0.0560(4) Uani d . 1 1 H H01 0.5771(12) 0.4699(7) 0.881(7) 0.058(5) Uiso d . 1 1 C C2 0.67226(12) 0.42632(9) 0.5609(6) 0.0757(5) Uani d . 1 1 H H2A 0.6340 0.3892 0.4536 0.114 Uiso calc R 1 1 H H2B 0.7234 0.4073 0.7130 0.114 Uiso calc R 1 1 H H2C 0.7193 0.4537 0.4247 0.114 Uiso calc R 1 1 O O1 0.5000 0.5000 0.2681(4) 0.0891(7) Uani d S 1 2 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 C1 0.0544(10) 0.0628(9) 0.0397(10) 0.0003(7) 0.000 0.000 N1 0.0548(6) 0.0683(6) 0.0448(7) 0.0073(4) 0.0024(5) 0.0014(6) C2 0.0640(8) 0.0845(9) 0.0787(11) 0.0158(7) 0.0134(8) 0.0003(9) O1 0.0930(12) 0.1358(17) 0.0385(10) 0.0295(12) 0.000 0.000 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O1 C1 N1 . 2_665 122.07(10) O1 C1 N1 . . 122.07(10) N1 C1 N1 2_665 . 115.87(19) C1 N1 C2 . . 122.36(16) C1 N1 H01 . . 116.6(10) C2 N1 H01 . . 120.3(10) 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 C1 O1 . 1.235(3) C1 N1 2_665 1.3434(16) C1 N1 . 1.3434(16) N1 C2 . 1.4394(19) N1 H01 . 0.85(3) 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 0.85(3) 2.06(3) 2.850(2) 154.4(14) 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_1 _geom_torsion O1 C1 N1 C2 . -7.54(14) N1 C1 N1 C2 2_665 172.46(14)