#------------------------------------------------------------------------------ #$Date: 2016-09-30 13:16:14 +0300 (Fri, 30 Sep 2016) $ #$Revision: 186852 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/42/1544224.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_1544224 loop_ _publ_author_name 'Olejniczak, Anna' 'Ostrowska, Kinga' 'Katrusiak, Andrzej' _publ_contact_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_email katran@amu.edu.pl _publ_contact_author_fax +48(61)8658008 _publ_contact_author_name 'Andrzej Katrusiak' _publ_contact_author_phone +48(61)8291443 _publ_section_title ; H-Bond Breaking in High-Pressure Urea ; _journal_issue 35 _journal_name_full 'The Journal of Physical Chemistry C' _journal_page_first 15761 _journal_paper_doi 10.1021/jp904942c _journal_volume 113 _journal_year 2009 _chemical_formula_moiety 'C H4 N2 O' _chemical_formula_sum 'C H4 N2 O' _chemical_formula_weight 60.06 _chemical_melting_point 405 _chemical_name_common urea _chemical_name_systematic ; urea ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _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 4 _cell_length_a 3.6235(11) _cell_length_b 8.272(4) _cell_length_c 8.844(4) _cell_measurement_pressure 800000 _cell_measurement_reflns_used 271 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 29.36 _cell_measurement_theta_min 3.37 _cell_volume 265.09(19) _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2002)' _computing_data_collection 'CrysAlis (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis (Oxford Diffraction, 2002)' _computing_molecular_graphics ;X-Seed (Barbour, 2001) and POV-Ray (Persistence of Vision, 2004) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 16.4 _diffrn_measured_fraction_theta_full 0.357 _diffrn_measured_fraction_theta_max 0.357 _diffrn_measurement_device_type 'Kuma KM4CCD \k geometry' _diffrn_measurement_method ;HP omega scans - for more details see: A. Budzianowski, A. Katrusiak in High-Pressure Crystallography (Eds.: A. Katrusiak, P. F. McMillan), Dordrecht: Kluwer Acad. Publ., 2004 pp.157-168 ; _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 0.0819 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 1790 _diffrn_reflns_theta_full 29.36 _diffrn_reflns_theta_max 29.36 _diffrn_reflns_theta_min 3.37 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; Katrusiak, A. (2003). REDSHABS - Program for correcting reflections intensities for DAC absorption, gasket shadowing and sample crystal absorption. Adam Mickiewicz University, Pozna\'n. Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 128 _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.153 _refine_diff_density_min -0.135 _refine_diff_density_rms 0.039 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -1(5) _refine_ls_extinction_coef 0.31(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 38 _refine_ls_number_reflns 271 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.187 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0538 _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^)+(0.0582P)^2^+0.0827P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1194 _refine_ls_wR_factor_ref 0.1215 _reflns_number_gt 251 _reflns_number_total 271 _reflns_threshold_expression >2sigma(I) _cod_data_source_file urea.cif _cod_data_source_block urea_080 _cod_original_cell_volume 265.09(18) _cod_database_code 1544224 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 N2 N 0.0976(8) 0.6314(5) 0.1147(4) 0.0395(12) Uani 1 1 d . . . H2A H -0.0018 0.7040 0.0582 0.047 Uiso 1 1 calc R . . H2B H 0.1570 0.6542 0.2064 0.047 Uiso 1 1 calc R . . C1 C 0.1608(9) 0.4811(6) 0.0591(6) 0.0291(12) Uani 1 1 d . . . O1 O 0.0768(7) 0.4456(4) -0.0736(3) 0.0382(11) Uani 1 1 d . . . N1 N 0.3248(9) 0.3759(6) 0.1518(4) 0.0372(12) Uani 1 1 d . . . H1A H 0.3760 0.2800 0.1206 0.045 Uiso 1 1 calc R . . H1B H 0.3793 0.4040 0.2427 0.045 Uiso 1 1 calc R . . 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 N2 0.046(2) 0.036(5) 0.037(4) -0.0033(15) -0.0061(16) 0.005(2) C1 0.0331(17) 0.022(6) 0.032(5) 0.0028(16) 0.0073(19) -0.0017(19) O1 0.0542(18) 0.028(4) 0.032(4) 0.0020(11) -0.0002(15) -0.0027(16) N1 0.053(2) 0.039(4) 0.020(4) -0.0015(12) -0.0012(17) 0.0062(18) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C1 N2 H2A 120.0 . . C1 N2 H2B 120.0 . . H2A N2 H2B 120.0 . . O1 C1 N1 122.2(5) . . O1 C1 N2 121.0(4) . . N1 C1 N2 116.8(6) . . C1 N1 H1A 120.0 . . C1 N1 H1B 120.0 . . H1A N1 H1B 120.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 N2 C1 1.357(7) . N2 H2A 0.8600 . N2 H2B 0.8600 . C1 O1 1.248(6) . C1 N1 1.335(6) . N1 H1A 0.8600 . N1 H1B 0.8600 .