#------------------------------------------------------------------------------ #$Date: 2013-02-21 00:16:41 +0200 (Thu, 21 Feb 2013) $ #$Revision: 73681 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/02/08/7020835.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_7020835 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 7.390(4) _cell_length_b 7.390(4) _cell_length_c 6.9266(19) _cell_measurement_pressure 960000 _cell_measurement_reflns_used 659 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 25.85 _cell_measurement_theta_min 4.03 _cell_volume 378.3(3) _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 0.424 _diffrn_measured_fraction_theta_max 0.424 _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 0.1385 _diffrn_reflns_av_sigmaI/netI 0.0450 _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 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 659 _diffrn_reflns_theta_full 25.85 _diffrn_reflns_theta_max 25.85 _diffrn_reflns_theta_min 4.03 _exptl_absorpt_coefficient_mu 1.682 _exptl_absorpt_correction_T_max 0.5891 _exptl_absorpt_correction_T_min 0.2547 _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 2.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate-shaped _exptl_crystal_F_000 272 _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _refine_diff_density_max 0.293 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.055 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.4(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.277 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 15 _refine_ls_number_reflns 50 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.277 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0380 _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^)+(0.0678P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.0849 _reflns_number_gt 50 _reflns_number_total 50 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c2dt32131a.txt _[local]_cod_data_source_block KDP_0.96GPa_CSD-424766 _[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 7020835 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 0.0244(11) Uani 1 4 d S P1 P 0.0000 0.0000 0.0000 0.0205(12) Uani 1 4 d S O1 O 0.15059(16) 0.0815(5) 0.1271(3) 0.0240(10) Uani 1 1 d . H1 H 0.1518 0.1917 0.1141 0.07(5) 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 0.0249(14) 0.0249(14) 0.0232(14) 0.000 0.000 0.000 P1 0.0187(15) 0.0187(15) 0.0241(16) 0.000 0.000 0.000 O1 0.0214(18) 0.0229(19) 0.0277(13) -0.0038(10) -0.005(2) 0.000(4) 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 95.36(3) 5 16_444 O1 K1 O1 95.36(3) 5 15_454 O1 K1 O1 144.39(9) 16_444 15_454 O1 K1 O1 144.39(9) 5 6_455 O1 K1 O1 95.36(3) 16_444 6_455 O1 K1 O1 95.36(3) 15_454 6_455 O1 K1 O1 132.73(4) 5 2 O1 K1 O1 67.36(5) 16_444 2 O1 K1 O1 80.55(6) 15_454 2 O1 K1 O1 82.56(6) 6_455 2 O1 K1 O1 80.55(6) 5 4_556 O1 K1 O1 132.73(4) 16_444 4_556 O1 K1 O1 82.56(6) 15_454 4_556 O1 K1 O1 67.36(5) 6_455 4_556 O1 K1 O1 143.75(5) 2 4_556 O1 K1 O1 67.36(5) 5 3_556 O1 K1 O1 82.56(6) 16_444 3_556 O1 K1 O1 132.73(4) 15_454 3_556 O1 K1 O1 80.55(6) 6_455 3_556 O1 K1 O1 143.75(5) 2 3_556 O1 K1 O1 52.20(7) 4_556 3_556 O1 K1 O1 82.56(6) 5 . O1 K1 O1 80.55(6) 16_444 . O1 K1 O1 67.36(5) 15_454 . O1 K1 O1 132.73(4) 6_455 . O1 K1 O1 52.20(7) 2 . O1 K1 O1 143.75(5) 4_556 . O1 K1 O1 143.75(5) 3_556 . O1 K1 P1 107.80(4) 5 . O1 K1 P1 72.20(4) 16_444 . O1 K1 P1 72.20(4) 15_454 . O1 K1 P1 107.80(4) 6_455 . O1 K1 P1 26.10(4) 2 . O1 K1 P1 153.90(4) 4_556 . O1 K1 P1 153.90(4) 3_556 . O1 K1 P1 26.10(4) . . O1 K1 P1 72.20(4) 5 1_556 O1 K1 P1 107.80(4) 16_444 1_556 O1 K1 P1 107.80(4) 15_454 1_556 O1 K1 P1 72.20(4) 6_455 1_556 O1 K1 P1 153.90(4) 2 1_556 O1 K1 P1 26.10(4) 4_556 1_556 O1 K1 P1 26.10(4) 3_556 1_556 O1 K1 P1 153.90(4) . 1_556 P1 K1 P1 180.0 . 1_556 O1 K1 K1 165.78(6) 5 5_455 O1 K1 K1 93.78(7) 16_444 5_455 O1 K1 K1 71.00(7) 15_454 5_455 O1 K1 K1 44.77(5) 6_455 5_455 O1 K1 K1 42.99(3) 2 5_455 O1 K1 K1 101.04(7) 4_556 5_455 O1 K1 K1 124.79(7) 3_556 5_455 O1 K1 K1 88.24(3) . 5_455 P1 K1 K1 64.891(13) . 5_455 P1 K1 K1 115.109(13) 1_556 5_455 O1 K1 K1 71.00(7) 5 13_455 O1 K1 K1 165.78(6) 16_444 13_455 O1 K1 K1 44.77(5) 15_454 13_455 O1 K1 K1 93.78(7) 6_455 13_455 O1 K1 K1 124.79(7) 2 13_455 O1 K1 K1 42.99(3) 4_556 13_455 O1 K1 K1 88.24(3) 3_556 13_455 O1 K1 K1 101.04(7) . 13_455 P1 K1 K1 115.109(13) . 13_455 P1 K1 K1 64.891(12) 1_556 13_455 K1 K1 K1 100.373(10) 5_455 13_455 O1 P1 O1 110.35(16) . 2 O1 P1 O1 109.03(8) . 4 O1 P1 O1 109.03(8) 2 4 O1 P1 O1 109.03(8) . 3 O1 P1 O1 109.03(8) 2 3 O1 P1 O1 110.35(16) 4 3 O1 P1 K1 124.82(8) . 1_554 O1 P1 K1 124.82(8) 2 1_554 O1 P1 K1 55.18(8) 4 1_554 O1 P1 K1 55.18(8) 3 1_554 O1 P1 K1 55.18(8) . . O1 P1 K1 55.18(8) 2 . O1 P1 K1 124.82(8) 4 . O1 P1 K1 124.82(8) 3 . K1 P1 K1 180.0 1_554 . P1 O1 K1 139.43(17) . 5 P1 O1 K1 98.73(10) . . K1 O1 K1 92.23(7) 5 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 K1 O1 2.785(2) 5 K1 O1 2.785(2) 16_444 K1 O1 2.785(2) 15_454 K1 O1 2.785(2) 6_455 K1 O1 2.876(2) 2 K1 O1 2.876(2) 4_556 K1 O1 2.876(2) 3_556 K1 O1 2.876(2) . K1 P1 3.4633(9) . K1 P1 3.4633(9) 1_556 K1 K1 4.0808(17) 5_455 K1 K1 4.0808(17) 13_455 P1 O1 1.5414(18) . P1 O1 1.5413(18) 2 P1 O1 1.5413(18) 4 P1 O1 1.5414(18) 3 P1 K1 3.4633(9) 1_554 O1 K1 2.785(2) 5