#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/67/2016712.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_2016712 loop_ _publ_author_name 'M\"uller, S.' 'Sch\"afer, O.' 'Keller, E.' _publ_section_title ; Rock salt--urea--water (1/1/1) at 293 and 117K ; _journal_coeditor_code GD3223 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m300 _journal_page_last m304 _journal_paper_doi 10.1107/S0108270108022427 _journal_volume 64 _journal_year 2008 _chemical_formula_iupac 'Na Cl, C H4 N2 O, H2 O' _chemical_formula_moiety 'Na Cl, C H4 N2 O, H2 O' _chemical_formula_sum 'C H6 Cl N2 Na O2' _chemical_formula_weight 136.52 _chemical_name_common 'rocksalt urea water' _chemical_name_systematic ; Rock salt--urea--water (1/1/1) (NaCl.CH~4~N~2~O.H~2~O) ; _space_group_IT_number 31 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P -2 -2bc' _symmetry_space_group_name_H-M 'P n 21 m' _atom_sites_solution_hydrogens difmap _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 6.4374(2) _cell_length_b 5.1744(2) _cell_length_c 17.2998(5) _cell_measurement_reflns_used 4386 _cell_measurement_temperature 117 _cell_measurement_theta_max 34.85 _cell_measurement_theta_min 2.35 _cell_volume 576.25(3) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_molecular_graphics 'SCHAKAL99 (Keller, 2004)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _diffrn_ambient_temperature 117 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker SMART 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 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 15591 _diffrn_reflns_theta_full 35.59 _diffrn_reflns_theta_max 35.59 _diffrn_reflns_theta_min 2.35 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'distorted cube' _exptl_crystal_F_000 280 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _refine_diff_density_max 0.660 _refine_diff_density_min -0.364 _refine_ls_abs_structure_details 'Flack (1983), 1109 Friedel pairs' _refine_ls_abs_structure_Flack -0.02(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 76 _refine_ls_number_reflns 2688 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 0.949 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0339 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.0859 _reflns_number_gt 2022 _reflns_number_total 2688 _reflns_threshold_expression >2sigma(I) _cod_data_source_file gd3223.cif _cod_data_source_block I_117K _cod_original_sg_symbol_H-M Pn21m _cod_database_code 2016712 _cod_database_fobs_code 2016712 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, y+1/2, z+1/2' 'x, y, -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 Cl Cl1 0.26051(4) 0.41551(8) 0.616725(17) 0.01411(8) Uani d . 1 Na Na1 0.51476(11) 0.19051(16) 0.5000 0.01254(17) Uani d S 1 Na Na2 -0.00615(11) 0.19552(16) 0.5000 0.01291(17) Uani d S 1 O O1 0.25054(19) -0.1198(3) 0.5000 0.0148(3) Uani d SD 1 H H1 0.236(2) -0.215(4) 0.5380(8) 0.030 Uiso d D 1 O O2 -0.2449(2) 0.5368(3) 0.5000 0.0142(3) Uani d SD 1 H H2 -0.234(2) 0.631(4) 0.5389(8) 0.028 Uiso d D 1 O O3 0.24513(15) 0.4920(2) 0.91144(6) 0.0143(2) Uani d . 1 N N1 0.1363(2) 0.6310(4) 0.79429(7) 0.0261(3) Uani d . 1 H H11 0.0490 0.7409 0.8155 0.031 Uiso calc R 1 H H12 0.1454 0.6201 0.7436 0.031 Uiso calc R 1 N N2 0.3852(2) 0.3192(4) 0.80336(7) 0.0265(3) Uani d . 1 H H21 0.4666 0.2178 0.8307 0.032 Uiso calc R 1 H H22 0.3897 0.3141 0.7525 0.032 Uiso calc R 1 C C1 0.2549(2) 0.4807(3) 0.83891(8) 0.0131(3) Uani d . 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 Cl1 0.01587(13) 0.01720(14) 0.00927(11) -0.0034(2) 0.00045(11) -0.00067(13) Na1 0.0095(3) 0.0144(4) 0.0136(4) -0.0007(3) 0.000 0.000 Na2 0.0102(3) 0.0155(4) 0.0130(4) -0.0004(3) 0.000 0.000 O1 0.0162(6) 0.0129(8) 0.0152(6) -0.0008(7) 0.000 0.000 O2 0.0170(7) 0.0122(7) 0.0133(6) -0.0004(6) 0.000 0.000 O3 0.0165(4) 0.0187(5) 0.0076(4) 0.0013(4) 0.0006(4) -0.0008(4) N1 0.0280(7) 0.0370(8) 0.0134(6) 0.0173(7) -0.0002(5) 0.0000(6) N2 0.0283(7) 0.0371(8) 0.0141(6) 0.0160(6) -0.0009(5) -0.0023(6) C1 0.0131(6) 0.0159(6) 0.0102(5) -0.0012(5) 0.0000(5) 0.0007(5) 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 _geom_angle_publ_flag Cl1 Na1 Cl1 4_556 . 90.31(3) ? Cl1 Na2 Cl1 . 4_556 88.86(3) ? Na1 Cl1 Na2 . . 71.60(2) no O1 Na1 O2 . 1_655 174.16(6) ? O1 Na1 O3 . 2_646 100.02(4) ? O2 Na1 O3 1_655 2_646 84.45(4) ? O3 Na1 O3 2_646 3_644 79.08(6) ? O1 Na1 Cl1 . 4_556 82.11(3) ? O2 Na1 Cl1 1_655 4_556 93.79(3) ? O3 Na1 Cl1 2_646 4_556 174.23(3) ? O3 Na1 Cl1 3_644 4_556 95.29(3) ? O2 Na1 Cl1 1_655 . 93.79(3) ? O1 Na2 O2 . . 175.67(6) ? O1 Na2 O3 . 3_544 98.45(5) ? O2 Na2 O3 . 3_544 84.88(4) ? O3 Na2 O3 3_544 2_546 78.83(6) ? O1 Na2 Cl1 . . 81.59(3) ? O2 Na2 Cl1 . . 95.34(3) ? O3 Na2 Cl1 3_544 . 174.94(4) ? O3 Na2 Cl1 2_546 . 96.15(3) ? Na2 O1 Na1 . . 92.01(6) no Na2 O2 Na1 . 1_455 81.84(6) no C1 O3 Na1 . 2_656 128.53(10) no C1 O3 Na2 . 2_556 133.28(10) no Na1 O3 Na2 2_656 2_556 79.57(4) no O3 C1 N2 . . 121.36(14) no O3 C1 N1 . . 121.40(14) no N2 C1 N1 . . 117.24(13) no H1 O1 H1 . 4_556 105(3) no H2 O2 H2 . 4_556 108(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 Na1 . 2.8481(7) yes Cl1 Na2 . 2.8845(7) yes Na1 Na2 1_655 3.0842(11) yes Na1 Na2 . 3.3534(11) yes Na1 O1 . 2.3392(16) yes Na1 O2 1_655 2.3674(17) yes Na1 O3 2_646 2.4066(12) yes Na2 O1 . 2.3223(16) yes Na2 O2 . 2.3411(17) yes Na2 O3 3_544 2.4131(12) yes O3 C1 . 1.2577(17) yes N1 C1 . 1.336(2) yes N2 C1 . 1.334(2) yes O1 H1 . 0.827(15) no O2 H2 . 0.833(15) no 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 H12 Cl1 . 0.88 2.55 3.3643(14) 154.7 N1 H11 Cl1 2_556 0.88 2.48 3.3260(14) 161.0 N2 H22 Cl1 . 0.88 2.55 3.3641(13) 154.8 N2 H21 Cl1 2_646 0.88 2.52 3.3877(15) 168.2 O1 H1 Cl1 1_545 0.827(15) 2.352(18) 3.1405(12) 159.5(19) O2 H2 O3 2_556 0.833(15) 2.06(2) 2.8097(18) 150(2)