#------------------------------------------------------------------------------ #$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $ #$Revision: 202017 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/25/7052510.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_7052510 loop_ _publ_author_name 'Andrew Parkin' 'Suzanne M. Harte' 'Andr\'es E. Goeta' 'Chick C. Wilson' _publ_section_title ; Imaging proton migration from X-rays and neutrons ; _journal_issue 6 _journal_name_full 'New J. Chem.' _journal_page_first 718 _journal_page_last 721 _journal_paper_doi 10.1039/b315515c _journal_volume 28 _journal_year 2004 _chemical_formula_moiety 'H2 O4 P, H, O C H4 N2' _chemical_formula_sum 'C H7 N2 O5 P' _chemical_formula_weight 158.06 _chemical_name_common '1:1 co-crystal of urea:phosphoric acid' _chemical_name_systematic ; ? ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary 'known coordinates' _atom_sites_solution_secondary none _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 7.4904(6) _cell_length_b 9.0176(7) _cell_length_c 17.7254(16) _cell_measurement_reflns_used 925 _cell_measurement_temperature 350(2) _cell_measurement_theta_max 25.94 _cell_measurement_theta_min 10.29 _cell_volume 1197.27(17) _computing_cell_refinement 'SMART V5.625 (Bruker, 2000)' _computing_data_collection 'SMART V5.625 (Bruker, 2000)' _computing_data_reduction 'SAINT V6.02A (Bruker, 2000)' _computing_molecular_graphics SHELXTL _computing_publication_material Encifer _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'known coordinates' _diffrn_ambient_temperature 350(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker SMART-6000 CCD Diffractometer' _diffrn_measurement_method '\w 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 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 7970 _diffrn_reflns_theta_full 30.52 _diffrn_reflns_theta_max 30.52 _diffrn_reflns_theta_min 2.30 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.419 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular shape' _exptl_crystal_F_000 656 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _refine_diff_density_max 0.283 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.146 _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 106 _refine_ls_number_reflns 1825 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.126 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0348 _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^)+(0.0598P)^2^+0.1712P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0955 _refine_ls_wR_factor_ref 0.1017 _reflns_number_gt 1548 _reflns_number_total 1825 _reflns_threshold_expression >2sigma(I) _cod_data_source_file b315515c.txt _cod_data_source_block 350k _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M Pbca _cod_database_code 7052510 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' '-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 P P 0.22188(5) 0.19112(3) 0.189146(17) 0.02807(13) Uani 1 1 d . . . O1 O 0.11640(12) 0.06527(9) 0.22252(5) 0.0332(2) Uani 1 1 d . . . O2 O 0.40893(14) 0.13983(13) 0.16078(6) 0.0411(3) Uani 1 1 d . . . H2 H 0.462(3) 0.115(3) 0.1964(13) 0.083(8) Uiso 1 1 d . . . O3 O 0.24872(18) 0.30662(12) 0.25283(6) 0.0412(3) Uani 1 1 d . . . H3 H 0.289(3) 0.380(3) 0.2424(11) 0.052(6) Uiso 1 1 d . . . O4 O 0.13430(15) 0.26158(12) 0.12068(5) 0.0409(3) Uani 1 1 d . . . O5 O -0.13406(16) 0.18945(10) 0.05344(7) 0.0439(3) Uani 1 1 d . . . N6 N -0.1382(2) -0.04150(16) 0.10362(8) 0.0496(4) Uani 1 1 d . . . H6A H -0.184(3) -0.132(3) 0.1033(11) 0.065(6) Uiso 1 1 d . . . H6B H -0.077(3) -0.014(3) 0.1390(11) 0.062(6) Uiso 1 1 d . . . N7 N -0.28227(19) 0.00983(16) -0.00695(8) 0.0439(3) Uani 1 1 d . . . H7A H -0.302(3) 0.078(2) -0.0422(10) 0.061(6) Uiso 1 1 d . . . H7B H -0.315(3) -0.074(2) -0.0092(12) 0.062(6) Uiso 1 1 d . . . C8 C -0.18332(18) 0.05346(14) 0.05054(7) 0.0326(3) Uani 1 1 d . . . H1 H -0.0030 0.2188 0.0913 0.040 Uani 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 P 0.0324(2) 0.02341(18) 0.02842(19) 0.00018(10) -0.00051(11) -0.00192(10) O1 0.0371(5) 0.0241(4) 0.0385(5) 0.0027(3) 0.0018(4) -0.0019(3) O2 0.0335(5) 0.0534(6) 0.0364(5) -0.0019(5) 0.0016(4) 0.0026(5) O3 0.0604(7) 0.0283(5) 0.0350(5) -0.0051(4) 0.0045(4) -0.0108(4) O4 0.0444(6) 0.0364(5) 0.0420(5) 0.0114(4) -0.0102(4) -0.0060(4) O5 0.0491(7) 0.0290(5) 0.0536(6) 0.0045(4) -0.0175(5) -0.0020(4) N6 0.0650(9) 0.0386(7) 0.0453(7) 0.0116(6) -0.0168(7) -0.0134(6) N7 0.0512(8) 0.0414(7) 0.0392(7) 0.0007(5) -0.0117(5) -0.0075(6) C8 0.0316(6) 0.0328(6) 0.0336(6) 0.0005(5) -0.0003(5) 0.0000(5) H1 0.047 0.030 0.044 0.008 0.005 0.003 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' P P 0.1023 0.0942 '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 _geom_angle_publ_flag O1 P O4 113.77(6) . . ? O1 P O3 106.79(6) . . ? O4 P O3 110.92(6) . . ? O1 P O2 112.03(6) . . ? O4 P O2 104.75(6) . . ? O3 P O2 108.53(7) . . ? P O2 H2 106.6(18) . . ? P O3 H3 117.8(16) . . ? P O4 H1 125.1 . . ? C8 O5 H1 117.5 . . ? C8 N6 H6A 119.7(13) . . ? C8 N6 H6B 119.8(16) . . ? H6A N6 H6B 120(2) . . ? C8 N7 H7A 115.5(13) . . ? C8 N7 H7B 119.5(16) . . ? H7A N7 H7B 125(2) . . ? O5 C8 N6 121.33(13) . . ? O5 C8 N7 118.53(13) . . ? N6 C8 N7 120.13(14) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P O1 1.5040(9) . ? P O4 1.5187(10) . ? P O3 1.5490(11) . ? P O2 1.5588(11) . ? O2 H2 0.78(2) . ? O3 H3 0.75(2) . ? O4 H1 1.2159 . ? O5 C8 1.2816(16) . ? O5 H1 1.2181 . ? N6 C8 1.3163(18) . ? N6 H6A 0.88(2) . ? N6 H6B 0.81(2) . ? N7 C8 1.3202(18) . ? N7 H7A 0.89(2) . ? N7 H7B 0.80(2) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H1 O4 1.22 1.22 2.4258(15) 170.6 . loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 19748