#------------------------------------------------------------------------------ #$Date: 2014-07-12 07:06:18 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/02/08/7020834.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_7020834 loop_ _publ_author_name 'Cai, Weizhao' 'Katrusiak, Andrzej' _publ_section_title ; Structure of the high-pressure phase IV of KH2PO4 (KDP). ; _journal_issue 4 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 863 _journal_page_last 866 _journal_volume 42 _journal_year 2013 _chemical_formula_moiety 'H2 O4 P, K' _chemical_formula_sum 'H2 K O4 P' _chemical_formula_weight 136.09 _chemical_name_common PotassiumDihydrogenPhosphate _chemical_name_systematic ; ? ; _space_group_IT_number 122 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I -4 2bw' _symmetry_space_group_name_H-M 'I -4 2 d' _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 7.455(8) _cell_length_b 7.455(8) _cell_length_c 6.947(2) _cell_measurement_pressure 210000 _cell_measurement_reflns_used 846 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.57 _cell_measurement_theta_min 4.10 _cell_volume 386.1(6) _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_collection 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.397 _diffrn_measured_fraction_theta_max 0.397 _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 0.2656 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 846 _diffrn_reflns_theta_full 27.57 _diffrn_reflns_theta_max 27.57 _diffrn_reflns_theta_min 4.01 _exptl_absorpt_coefficient_mu 1.649 _exptl_absorpt_correction_T_max 0.6777 _exptl_absorpt_correction_T_min 0.3027 _exptl_absorpt_correction_type analytical _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 2.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate-shaped _exptl_crystal_F_000 272 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.269 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.061 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.3(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 15 _refine_ls_number_reflns 56 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.023 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0418 _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^)+(0.0407P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.0727 _reflns_number_gt 39 _reflns_number_total 56 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c2dt32131a.txt _[local]_cod_data_source_block KDP_0.21GPa_CSD-424765 _[local]_cod_cif_authors_sg_H-M I-42d _[local]_cod_cif_authors_sg_Hall 'I -4 2bw ' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius ; _cod_database_code 7020834 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' 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 K1 K 0.0000 0.0000 0.5000 0.0300(11) Uani 1 4 d S P1 P 0.0000 0.0000 0.0000 0.0253(12) Uani 1 4 d S O1 O 0.1499(7) 0.0826(6) 0.1263(5) 0.0290(10) Uani 1 1 d . H1 H 0.1492 0.1920 0.1142 0.03(4) Uiso 0.50 1 calc PR 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 K1 0.0348(15) 0.0348(15) 0.0205(10) 0.000 0.000 0.000 P1 0.0283(17) 0.0283(17) 0.0195(11) 0.000 0.000 0.000 O1 0.031(2) 0.032(2) 0.0246(13) -0.0045(18) -0.001(3) 0.001(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 O1 K1 O1 144.46(16) 5 6_455 O1 K1 O1 95.34(5) 5 16_444 O1 K1 O1 95.34(5) 6_455 16_444 O1 K1 O1 95.34(5) 5 15_454 O1 K1 O1 95.34(5) 6_455 15_454 O1 K1 O1 144.46(16) 16_444 15_454 O1 K1 O1 132.72(12) 5 2 O1 K1 O1 82.50(13) 6_455 2 O1 K1 O1 67.25(8) 16_444 2 O1 K1 O1 80.73(12) 15_454 2 O1 K1 O1 80.73(12) 5 4_556 O1 K1 O1 67.25(8) 6_455 4_556 O1 K1 O1 132.72(12) 16_444 4_556 O1 K1 O1 82.50(13) 15_454 4_556 O1 K1 O1 143.66(12) 2 4_556 O1 K1 O1 67.25(8) 5 3_556 O1 K1 O1 80.73(12) 6_455 3_556 O1 K1 O1 82.50(13) 16_444 3_556 O1 K1 O1 132.72(12) 15_454 3_556 O1 K1 O1 143.66(12) 2 3_556 O1 K1 O1 52.33(18) 4_556 3_556 O1 K1 O1 82.50(13) 5 . O1 K1 O1 132.72(12) 6_455 . O1 K1 O1 80.73(12) 16_444 . O1 K1 O1 67.25(8) 15_454 . O1 K1 O1 52.33(18) 2 . O1 K1 O1 143.66(12) 4_556 . O1 K1 O1 143.66(12) 3_556 . O1 K1 P1 107.77(8) 5 . O1 K1 P1 107.77(8) 6_455 . O1 K1 P1 72.23(8) 16_444 . O1 K1 P1 72.23(8) 15_454 . O1 K1 P1 26.16(9) 2 . O1 K1 P1 153.84(9) 4_556 . O1 K1 P1 153.84(9) 3_556 . O1 K1 P1 26.16(9) . . O1 K1 P1 72.23(8) 5 1_556 O1 K1 P1 72.23(8) 6_455 1_556 O1 K1 P1 107.77(8) 16_444 1_556 O1 K1 P1 107.77(8) 15_454 1_556 O1 K1 P1 153.84(9) 2 1_556 O1 K1 P1 26.16(9) 4_556 1_556 O1 K1 P1 26.16(9) 3_556 1_556 O1 K1 P1 153.84(9) . 1_556 P1 K1 P1 180.0 . 1_556 O1 K1 K1 165.70(9) 5 5_455 O1 K1 K1 44.66(8) 6_455 5_455 O1 K1 K1 93.97(9) 16_444 5_455 O1 K1 K1 70.91(9) 15_454 5_455 O1 K1 K1 43.19(10) 2 5_455 O1 K1 K1 100.73(10) 4_556 5_455 O1 K1 K1 124.89(10) 3_556 5_455 O1 K1 K1 88.34(10) . 5_455 P1 K1 K1 65.02(2) . 5_455 P1 K1 K1 114.98(2) 1_556 5_455 O1 K1 K1 70.91(9) 5 13_455 O1 K1 K1 93.97(9) 6_455 13_455 O1 K1 K1 165.70(9) 16_444 13_455 O1 K1 K1 44.66(9) 15_454 13_455 O1 K1 K1 124.89(10) 2 13_455 O1 K1 K1 43.19(10) 4_556 13_455 O1 K1 K1 88.34(10) 3_556 13_455 O1 K1 K1 100.73(10) . 13_455 P1 K1 K1 114.98(2) . 13_455 P1 K1 K1 65.02(2) 1_556 13_455 K1 K1 K1 100.276(18) 5_455 13_455 O1 P1 O1 108.74(14) . 3 O1 P1 O1 108.74(14) . 4 O1 P1 O1 111.0(3) 3 4 O1 P1 O1 111.0(3) . 2 O1 P1 O1 108.74(14) 3 2 O1 P1 O1 108.74(14) 4 2 O1 P1 K1 55.48(14) . . O1 P1 K1 124.52(14) 3 . O1 P1 K1 124.52(14) 4 . O1 P1 K1 55.48(14) 2 . O1 P1 K1 124.52(14) . 1_554 O1 P1 K1 55.48(14) 3 1_554 O1 P1 K1 55.48(14) 4 1_554 O1 P1 K1 124.52(14) 2 1_554 K1 P1 K1 180.0 . 1_554 P1 O1 K1 139.0(3) . 5 P1 O1 K1 98.36(19) . . K1 O1 K1 92.15(13) 5 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 K1 O1 2.816(6) 5 K1 O1 2.816(6) 6_455 K1 O1 2.816(6) 16_444 K1 O1 2.816(6) 15_454 K1 O1 2.893(4) 2 K1 O1 2.893(4) 4_556 K1 O1 2.893(4) 3_556 K1 O1 2.893(4) . K1 P1 3.4736(10) . K1 P1 3.4736(10) 1_556 K1 K1 4.112(4) 5_455 K1 K1 4.112(3) 13_455 P1 O1 1.548(4) . P1 O1 1.548(4) 3 P1 O1 1.548(4) 4 P1 O1 1.548(4) 2 P1 K1 3.4736(10) 1_554 O1 K1 2.816(6) 5 _journal_paper_doi 10.1039/c2dt32131a