data_KDP_0.21GPa CSD-424765 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Andrzej Katrusiak' _publ_contact_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_fax '+48(61)8291505' _publ_contact_author_phone '+48(61)8291443' _publ_contact_author_email katran@amu.edu.pl _publ_section_title ; ? ; loop_ _publ_author_footnote ; Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _chemical_name_systematic ; ? ; _chemical_name_common PotassiumDihydrogenPhosphate _chemical_melting_point ? _chemical_formula_moiety 'H2 O4 P, K' _chemical_formula_sum 'H2 K O4 P' _chemical_formula_weight 136.09 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I -4 2bw ' 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' _cell_length_a 7.455(8) _cell_length_b 7.455(8) _cell_length_c 6.947(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 386.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_pressure 210000 _cell_measurement_reflns_used 846 _cell_measurement_theta_min 4.10 _cell_measurement_theta_max 27.57 _exptl_crystal_description 'plate-shaped' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 272 _exptl_absorpt_coefficient_mu 1.649 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.3027 _exptl_absorpt_correction_T_max 0.6777 _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_special_details ; Data were collected at room temperature and pressure of 0.21(3) GPa (210000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _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_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 846 _diffrn_reflns_av_R_equivalents 0.2656 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 27.57 _reflns_number_total 56 _reflns_number_gt 39 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.3(4) _refine_ls_number_reflns 56 _refine_ls_number_parameters 15 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 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) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 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 ? 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 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 . ? _diffrn_measured_fraction_theta_max 0.397 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.397 _refine_diff_density_max 0.269 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.061 #===END data_KDP_0.96GPa CSD-424766 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Andrzej Katrusiak' _publ_contact_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_fax '+48(61)8291505' _publ_contact_author_phone '+48(61)8291443' _publ_contact_author_email katran@amu.edu.pl _publ_section_title ; ? ; loop_ _publ_author_footnote ; Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _chemical_name_systematic ; ? ; _chemical_name_common PotassiumDihydrogenPhosphate _chemical_melting_point ? _chemical_formula_moiety 'H2 O4 P, K' _chemical_formula_sum 'H2 K O4 P' _chemical_formula_weight 136.09 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I -4 2bw ' 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' _cell_length_a 7.390(4) _cell_length_b 7.390(4) _cell_length_c 6.9266(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 378.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_pressure 960000 _cell_measurement_reflns_used 659 _cell_measurement_theta_min 4.03 _cell_measurement_theta_max 25.85 _exptl_crystal_description 'plate-shaped' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 272 _exptl_absorpt_coefficient_mu 1.682 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.2547 _exptl_absorpt_correction_T_max 0.5891 _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_special_details ; Data were collected at room temperature and pressure of 0.96(3) GPa (960000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _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_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 659 _diffrn_reflns_av_R_equivalents 0.1385 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 25.85 _reflns_number_total 50 _reflns_number_gt 50 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.4(3) _refine_ls_number_reflns 50 _refine_ls_number_parameters 15 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.277 _refine_ls_restrained_S_all 1.277 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 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) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 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 ? 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 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 . ? _diffrn_measured_fraction_theta_max 0.424 _diffrn_reflns_theta_full 25.85 _diffrn_measured_fraction_theta_full 0.424 _refine_diff_density_max 0.293 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.055 #===END data_KDP_1.11GPa CSD-424767 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Andrzej Katrusiak' _publ_contact_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_fax '+48(61)8291505' _publ_contact_author_phone '+48(61)8291443' _publ_contact_author_email katran@amu.edu.pl _publ_section_title ; ? ; loop_ _publ_author_footnote ; Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _chemical_name_systematic ; ? ; _chemical_name_common PotassiumDihydrogenPhosphate _chemical_melting_point ? _chemical_formula_moiety 'H2 O4 P, K' _chemical_formula_sum 'H2 K O4 P' _chemical_formula_weight 136.09 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall "-P 2ybc" loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.148(5) _cell_length_b 4.484(11) _cell_length_c 13.909(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.53(7) _cell_angle_gamma 90.00 _cell_volume 383.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_pressure 1110000 _cell_measurement_reflns_used 1063 _cell_measurement_theta_min 4.48 _cell_measurement_theta_max 28.55 _exptl_crystal_description 'triangle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 272 _exptl_absorpt_coefficient_mu 1.661 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.3528 _exptl_absorpt_correction_T_max 0.6577 _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_special_details ; Data were collected at room temperature and pressure of 1.11(3) GPa (1110000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _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_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1063 _diffrn_reflns_av_R_equivalents 0.2501 _diffrn_reflns_av_sigmaI/netI 0.1382 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.48 _diffrn_reflns_theta_max 28.55 _reflns_number_total 172 _reflns_number_gt 147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Due to the limited diffraction data, the anisotropic values of K1, P1, O1, O2, O3 and O4 atoms were restrained to approximate isotropic shape by using command ISOR 0.01 of SHELXL-97. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+4.4679P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 172 _refine_ls_number_parameters 56 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1589 _refine_ls_R_factor_gt 0.1368 _refine_ls_wR_factor_ref 0.2888 _refine_ls_wR_factor_gt 0.2738 _refine_ls_goodness_of_fit_ref 1.388 _refine_ls_restrained_S_all 1.261 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 K1 K 0.7622(8) 0.508(3) 0.6259(3) 0.033(4) Uani 1 1 d U . . P1 P 0.7468(12) 0.480(5) 0.8713(5) 0.052(5) Uani 1 1 d U . . O1 O 0.662(2) 0.165(8) 0.8040(9) 0.022(5) Uani 1 1 d U . . H1 H 0.7433 -0.0314 0.8054 0.034 Uiso 1 1 d . . . O2 O 0.849(3) 0.707(14) 0.8076(13) 0.067(7) Uani 1 1 d U . . O3 O 0.542(2) 0.603(9) 0.9223(9) 0.036(6) Uani 1 1 d U . . H2 H 0.5290 0.5182 0.9741 0.054 Uiso 0.50 1 calc PR . . O4 O 0.8972(17) 0.257(11) 0.9373(7) 0.018(5) Uani 1 1 d U . . H3 H 0.9671 0.3542 0.9773 0.027 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 0.030(3) 0.036(13) 0.035(3) 0.006(3) 0.006(2) -0.009(4) P1 0.048(4) 0.054(13) 0.053(4) 0.005(6) -0.008(4) 0.007(6) O1 0.016(5) 0.023(13) 0.027(6) -0.001(8) -0.019(5) 0.006(9) O2 0.062(9) 0.067(14) 0.072(8) 0.002(10) -0.006(7) 0.003(10) O3 0.036(7) 0.035(14) 0.037(7) 0.002(8) 0.015(5) 0.004(9) O4 0.013(5) 0.017(13) 0.025(5) -0.003(8) 0.012(4) 0.003(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 K1 O4 2.55(2) 2_756 ? K1 O3 2.68(3) 2_646 ? K1 O2 2.72(3) . ? K1 O2 2.88(3) 2_746 ? K1 O1 2.897(17) 2_656 ? K1 O1 2.99(2) . ? K1 O4 3.02(2) 4_565 ? K1 O3 3.31(4) 2_656 ? K1 P1 3.419(9) . ? K1 P1 3.684(16) 2_756 ? K1 P1 3.778(17) 2_656 ? K1 P1 3.837(18) 2_746 ? P1 O2 1.50(5) . ? P1 O3 1.56(2) . ? P1 O4 1.63(4) . ? P1 O1 1.76(4) . ? P1 K1 3.684(16) 2_746 ? P1 K1 3.778(17) 2_646 ? P1 K1 3.837(18) 2_756 ? O1 K1 2.897(17) 2_646 ? O2 K1 2.88(3) 2_756 ? O3 K1 2.68(3) 2_656 ? O3 K1 3.31(4) 2_646 ? O4 K1 2.55(2) 2_746 ? O4 K1 3.02(2) 4_566 ? 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 O4 K1 O3 141.6(7) 2_756 2_646 ? O4 K1 O2 92.0(9) 2_756 . ? O3 K1 O2 125.0(10) 2_646 . ? O4 K1 O2 68.5(12) 2_756 2_746 ? O3 K1 O2 109.2(14) 2_646 2_746 ? O2 K1 O2 73.4(5) . 2_746 ? O4 K1 O1 140.0(15) 2_756 2_656 ? O3 K1 O1 67.7(9) 2_646 2_656 ? O2 K1 O1 76.4(5) . 2_656 ? O2 K1 O1 139.0(6) 2_746 2_656 ? O4 K1 O1 134.3(5) 2_756 . ? O3 K1 O1 72.6(6) 2_646 . ? O2 K1 O1 55.8(12) . . ? O2 K1 O1 71.3(7) 2_746 . ? O1 K1 O1 68.9(3) 2_656 . ? O4 K1 O4 67.9(13) 2_756 4_565 ? O3 K1 O4 73.8(7) 2_646 4_565 ? O2 K1 O4 152.3(6) . 4_565 ? O2 K1 O4 81.3(8) 2_746 4_565 ? O1 K1 O4 131.2(4) 2_656 4_565 ? O1 K1 O4 125.7(10) . 4_565 ? O4 K1 O3 92.5(10) 2_756 2_656 ? O3 K1 O3 96.2(5) 2_646 2_656 ? O2 K1 O3 91.2(12) . 2_656 ? O2 K1 O3 154.5(13) 2_746 2_656 ? O1 K1 O3 50.5(7) 2_656 2_656 ? O1 K1 O3 117.0(6) . 2_656 ? O4 K1 O3 107.9(8) 4_565 2_656 ? O4 K1 P1 113.9(4) 2_756 . ? O3 K1 P1 100.8(5) 2_646 . ? O2 K1 P1 25.1(11) . . ? O2 K1 P1 72.9(4) 2_746 . ? O1 K1 P1 67.9(3) 2_656 . ? O1 K1 P1 31.0(7) . . ? O4 K1 P1 150.3(9) 4_565 . ? O3 K1 P1 101.6(4) 2_656 . ? O4 K1 P1 22.0(6) 2_756 2_756 ? O3 K1 P1 163.2(4) 2_646 2_756 ? O2 K1 P1 70.3(9) . 2_756 ? O2 K1 P1 66.0(11) 2_746 2_756 ? O1 K1 P1 127.1(7) 2_656 2_756 ? O1 K1 P1 118.2(4) . 2_756 ? O4 K1 P1 89.5(6) 4_565 2_756 ? O3 K1 P1 89.9(6) 2_656 2_756 ? P1 K1 P1 93.2(3) . 2_756 ? O4 K1 P1 116.6(11) 2_756 2_656 ? O3 K1 P1 79.0(7) 2_646 2_656 ? O2 K1 P1 87.1(8) . 2_656 ? O2 K1 P1 160.3(7) 2_746 2_656 ? O1 K1 P1 26.7(6) 2_656 2_656 ? O1 K1 P1 95.2(5) . 2_656 ? O4 K1 P1 118.5(5) 4_565 2_656 ? O3 K1 P1 24.3(4) 2_656 2_656 ? P1 K1 P1 88.0(3) . 2_656 ? P1 K1 P1 111.0(7) 2_756 2_656 ? O4 K1 P1 67.7(10) 2_756 2_746 ? O3 K1 P1 97.3(8) 2_646 2_746 ? O2 K1 P1 93.3(8) . 2_746 ? O2 K1 P1 19.9(7) 2_746 2_746 ? O1 K1 P1 149.6(7) 2_656 2_746 ? O1 K1 P1 81.5(5) . 2_746 ? O4 K1 P1 62.0(5) 4_565 2_746 ? O3 K1 P1 159.8(5) 2_656 2_746 ? P1 K1 P1 90.6(3) . 2_746 ? P1 K1 P1 73.2(2) 2_756 2_746 ? P1 K1 P1 175.7(6) 2_656 2_746 ? O2 P1 O3 113(2) . . ? O2 P1 O4 120.6(13) . . ? O3 P1 O4 114.4(11) . . ? O2 P1 O1 110.6(17) . . ? O3 P1 O1 107.1(14) . . ? O4 P1 O1 88(2) . . ? O2 P1 K1 50.3(14) . . ? O3 P1 K1 118.9(8) . . ? O4 P1 K1 123.7(10) . . ? O1 P1 K1 61.0(7) . . ? O2 P1 K1 92.2(14) . 2_746 ? O3 P1 K1 150.2(11) . 2_746 ? O4 P1 K1 35.8(5) . 2_746 ? O1 P1 K1 77.1(9) . 2_746 ? K1 P1 K1 89.3(3) . 2_746 ? O2 P1 K1 138.3(8) . 2_646 ? O3 P1 K1 61.0(13) . 2_646 ? O4 P1 K1 96.2(14) . 2_646 ? O1 P1 K1 47.6(5) . 2_646 ? K1 P1 K1 94.4(3) . 2_646 ? K1 P1 K1 111.0(7) 2_746 2_646 ? O2 P1 K1 40.9(8) . 2_756 ? O3 P1 K1 114.9(15) . 2_756 ? O4 P1 K1 86.5(12) . 2_756 ? O1 P1 K1 136.0(5) . 2_756 ? K1 P1 K1 86.8(3) . 2_756 ? K1 P1 K1 73.2(2) 2_746 2_756 ? K1 P1 K1 175.7(6) 2_646 2_756 ? P1 O1 K1 105.7(8) . 2_646 ? P1 O1 K1 87.9(12) . . ? K1 O1 K1 127.6(5) 2_646 . ? P1 O2 K1 105(2) . . ? P1 O2 K1 119.2(10) . 2_756 ? K1 O2 K1 126.4(9) . 2_756 ? P1 O3 K1 133.7(13) . 2_656 ? P1 O3 K1 94.6(16) . 2_646 ? K1 O3 K1 96.2(5) 2_656 2_646 ? P1 O4 K1 122.2(6) . 2_746 ? P1 O4 K1 124.5(7) . 4_566 ? K1 O4 K1 112.1(13) 2_746 4_566 ? _diffrn_measured_fraction_theta_max 0.176 _diffrn_reflns_theta_full 28.55 _diffrn_measured_fraction_theta_full 0.176 _refine_diff_density_max 0.259 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.069 #===END data_KDP_1.46GPa CSD-424768 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Andrzej Katrusiak' _publ_contact_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_fax '+48(61)8291505' _publ_contact_author_phone '+48(61)8291443' _publ_contact_author_email katran@amu.edu.pl _publ_section_title ; ? ; loop_ _publ_author_footnote ; Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _chemical_name_systematic ; ? ; _chemical_name_common PotassiumDihydrogenPhosphate _chemical_melting_point ? _chemical_formula_moiety 'H2 O4 P, K' _chemical_formula_sum 'H2 K O4 P' _chemical_formula_weight 136.09 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I -4 2bw ' 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' _cell_length_a 7.366(4) _cell_length_b 7.366(4) _cell_length_c 6.8894(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 373.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_pressure 1460000 _cell_measurement_reflns_used 760 _cell_measurement_theta_min 4.05 _cell_measurement_theta_max 27.82 _exptl_crystal_description 'plate-shaped' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 272 _exptl_absorpt_coefficient_mu 1.703 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.2818 _exptl_absorpt_correction_T_max 0.5983 _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_special_details ; Data were collected at room temperature and pressure of 1.46(3) GPa (1460000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _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_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 760 _diffrn_reflns_av_R_equivalents 0.1512 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.05 _diffrn_reflns_theta_max 27.82 _reflns_number_total 48 _reflns_number_gt 48 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+0.2412P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.3(3) _refine_ls_number_reflns 48 _refine_ls_number_parameters 15 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 K1 K 0.0000 0.0000 0.5000 0.0229(12) Uani 1 4 d S . . P1 P 0.0000 0.0000 0.0000 0.0199(13) Uani 1 4 d S . . O1 O 0.1518(3) 0.0810(6) 0.1280(4) 0.0230(13) Uani 1 1 d . . . H1 H 0.1528 0.1918 0.1161 0.02(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 0.0247(16) 0.0247(16) 0.0192(14) 0.000 0.000 0.000 P1 0.0194(17) 0.0194(17) 0.0209(15) 0.000 0.000 0.000 O1 0.0210(19) 0.022(2) 0.0260(16) -0.0039(14) -0.006(3) 0.000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 K1 O1 2.764(3) 5 ? K1 O1 2.764(3) 16_444 ? K1 O1 2.764(3) 6_455 ? K1 O1 2.764(3) 15_454 ? K1 O1 2.859(3) 2 ? K1 O1 2.859(3) 4_556 ? K1 O1 2.859(3) 3_556 ? K1 O1 2.859(3) . ? K1 P1 3.4447(9) . ? K1 P1 3.4447(9) 1_556 ? K1 K1 4.0656(17) 5_455 ? K1 K1 4.0656(17) 13_455 ? P1 O1 1.544(3) . ? P1 O1 1.544(3) 3 ? P1 O1 1.544(3) 2 ? P1 O1 1.544(3) 4 ? P1 K1 3.4447(9) 1_554 ? O1 K1 2.764(3) 5 ? 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 K1 O1 95.31(4) 5 16_444 ? O1 K1 O1 144.60(13) 5 6_455 ? O1 K1 O1 95.31(4) 16_444 6_455 ? O1 K1 O1 95.31(4) 5 15_454 ? O1 K1 O1 144.60(13) 16_444 15_454 ? O1 K1 O1 95.31(4) 6_455 15_454 ? O1 K1 O1 132.88(7) 5 2 ? O1 K1 O1 67.56(7) 16_444 2 ? O1 K1 O1 82.22(9) 6_455 2 ? O1 K1 O1 80.60(9) 15_454 2 ? O1 K1 O1 80.60(9) 5 4_556 ? O1 K1 O1 132.88(7) 16_444 4_556 ? O1 K1 O1 67.56(7) 6_455 4_556 ? O1 K1 O1 82.22(9) 15_454 4_556 ? O1 K1 O1 143.46(7) 2 4_556 ? O1 K1 O1 67.56(7) 5 3_556 ? O1 K1 O1 82.22(9) 16_444 3_556 ? O1 K1 O1 80.60(9) 6_455 3_556 ? O1 K1 O1 132.88(7) 15_454 3_556 ? O1 K1 O1 143.46(7) 2 3_556 ? O1 K1 O1 52.63(10) 4_556 3_556 ? O1 K1 O1 82.22(9) 5 . ? O1 K1 O1 80.60(9) 16_444 . ? O1 K1 O1 132.88(7) 6_455 . ? O1 K1 O1 67.56(7) 15_454 . ? O1 K1 O1 52.63(10) 2 . ? O1 K1 O1 143.46(7) 4_556 . ? O1 K1 O1 143.46(7) 3_556 . ? O1 K1 P1 107.70(6) 5 . ? O1 K1 P1 72.30(6) 16_444 . ? O1 K1 P1 107.70(6) 6_455 . ? O1 K1 P1 72.30(6) 15_454 . ? O1 K1 P1 26.31(5) 2 . ? O1 K1 P1 153.69(5) 4_556 . ? O1 K1 P1 153.69(5) 3_556 . ? O1 K1 P1 26.31(5) . . ? O1 K1 P1 72.30(6) 5 1_556 ? O1 K1 P1 107.70(6) 16_444 1_556 ? O1 K1 P1 72.30(6) 6_455 1_556 ? O1 K1 P1 107.70(6) 15_454 1_556 ? O1 K1 P1 153.69(5) 2 1_556 ? O1 K1 P1 26.31(5) 4_556 1_556 ? O1 K1 P1 26.31(5) 3_556 1_556 ? O1 K1 P1 153.69(5) . 1_556 ? P1 K1 P1 180.0 . 1_556 ? O1 K1 K1 165.77(8) 5 5_455 ? O1 K1 K1 93.82(9) 16_444 5_455 ? O1 K1 K1 44.63(7) 6_455 5_455 ? O1 K1 K1 71.08(9) 15_454 5_455 ? O1 K1 K1 42.78(5) 2 5_455 ? O1 K1 K1 101.00(9) 4_556 5_455 ? O1 K1 K1 124.66(9) 3_556 5_455 ? O1 K1 K1 88.54(5) . 5_455 ? P1 K1 K1 64.936(12) . 5_455 ? P1 K1 K1 115.064(12) 1_556 5_455 ? O1 K1 K1 71.07(9) 5 13_455 ? O1 K1 K1 165.77(8) 16_444 13_455 ? O1 K1 K1 93.82(9) 6_455 13_455 ? O1 K1 K1 44.63(7) 15_454 13_455 ? O1 K1 K1 124.66(9) 2 13_455 ? O1 K1 K1 42.78(5) 4_556 13_455 ? O1 K1 K1 88.54(5) 3_556 13_455 ? O1 K1 K1 101.00(9) . 13_455 ? P1 K1 K1 115.064(12) . 13_455 ? P1 K1 K1 64.936(12) 1_556 13_455 ? K1 K1 K1 100.339(10) 5_455 13_455 ? O1 P1 O1 109.04(11) . 3 ? O1 P1 O1 110.3(2) . 2 ? O1 P1 O1 109.04(11) 3 2 ? O1 P1 O1 109.04(11) . 4 ? O1 P1 O1 110.3(2) 3 4 ? O1 P1 O1 109.04(11) 2 4 ? O1 P1 K1 124.83(12) . 1_554 ? O1 P1 K1 55.17(12) 3 1_554 ? O1 P1 K1 124.83(12) 2 1_554 ? O1 P1 K1 55.17(12) 4 1_554 ? O1 P1 K1 55.17(12) . . ? O1 P1 K1 124.83(12) 3 . ? O1 P1 K1 55.17(12) 2 . ? O1 P1 K1 124.83(12) 4 . ? K1 P1 K1 180.0 1_554 . ? P1 O1 K1 139.7(2) . 5 ? P1 O1 K1 98.52(13) . . ? K1 O1 K1 92.60(10) 5 . ? _diffrn_measured_fraction_theta_max 0.340 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.340 _refine_diff_density_max 0.223 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.050 #===END data_KDP_1.62GPa CSD-424769 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Andrzej Katrusiak' _publ_contact_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_fax '+48(61)8291505' _publ_contact_author_phone '+48(61)8291443' _publ_contact_author_email katran@amu.edu.pl _publ_section_title ; ? ; loop_ _publ_author_footnote ; Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _chemical_name_systematic ; ? ; _chemical_name_common PotassiumDihydrogenPhosphate _chemical_melting_point ? _chemical_formula_moiety 'H2 O4 P, K' _chemical_formula_sum 'H2 K O4 P' _chemical_formula_weight 136.09 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall "-P 2ybc" loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.384(3) _cell_length_b 4.449(5) _cell_length_c 18.305(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.11(2) _cell_angle_gamma 90.00 _cell_volume 1113.3(13) _cell_formula_units_Z 12 _cell_measurement_temperature 296(2) _cell_measurement_pressure 1620000 _cell_measurement_reflns_used 2744 _cell_measurement_theta_min 4.33 _cell_measurement_theta_max 26.51 _exptl_crystal_description 'plate-like' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.715 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.4226 _exptl_absorpt_correction_T_max 0.6740 _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_special_details ; Data were collected at room temperature and pressure of 1.62(3) GPa (1620000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _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_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2744 _diffrn_reflns_av_R_equivalents 0.1223 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.33 _diffrn_reflns_theta_max 26.51 _reflns_number_total 440 _reflns_number_gt 390 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Due to the limited diffraction data,the anisotropic values of all K, P and O atoms All atoms were restrained to approximate isotropic shape by using command ISOR 0.01 of SHELXL-97 except O6 and O11 atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1557P)^2^+2.0468P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 440 _refine_ls_number_parameters 163 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.2004 _refine_ls_wR_factor_gt 0.1865 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 K1 K 0.1592(2) 0.0601(16) 0.26455(15) 0.033(4) Uani 1 1 d U . . K2 K 0.1803(2) -0.0348(16) 0.02545(16) 0.041(4) Uani 1 1 d U . . K3 K 0.5067(2) 0.0124(15) 0.13358(16) 0.033(4) Uani 1 1 d U . . P1 P 0.3275(2) 0.5162(18) 0.1869(2) 0.030(4) Uani 1 1 d U . . P2 P 0.3345(2) 0.0753(19) 0.4350(2) 0.030(4) Uani 1 1 d U . . P3 P 0.0167(2) 0.108(2) 0.38122(18) 0.024(4) Uani 1 1 d U . . O1 O 0.3986(7) 0.284(7) 0.2225(5) 0.050(5) Uani 1 1 d U . . H1 H 0.3735 0.0799 0.2321 0.060 Uiso 0.50 1 d P . . O5 O 0.2571(6) -0.148(6) 0.4119(5) 0.038(5) Uani 1 1 d U . . H5 H 0.2781 -0.3621 0.3983 0.045 Uiso 0.50 1 d P . . O9 O 0.0838(6) 0.349(6) 0.3710(5) 0.045(5) Uani 1 1 d U . . H9 H 0.0573 0.5574 0.3516 0.054 Uiso 0.50 1 d P . . O2 O 0.2234(6) 0.394(4) 0.1609(5) 0.035(4) Uani 1 1 d U . . H2 H 0.1660 0.5371 0.1486 0.042 Uiso 0.50 1 d P . . O6 O 0.3087(5) 0.319(6) 0.3762(5) 0.038(16) Uani 1 1 d . . . H6 H 0.2890 -0.4742 0.3906 0.045 Uiso 0.50 1 d P . . O10 O 0.0160(6) -0.125(6) 0.3224(5) 0.042(5) Uani 1 1 d U . . H10 H 0.0426 0.6720 0.3408 0.051 Uiso 0.50 1 d P . . O3 O 0.3533(6) 0.652(6) 0.1182(4) 0.040(5) Uani 1 1 d U . . H3 H 0.3463 0.5095 0.0745 0.048 Uiso 0.50 1 d P . . O4 O 0.3332(6) 0.757(6) 0.2465(5) 0.041(4) Uani 1 1 d U . . H4 H 0.3584 -0.0416 0.2377 0.049 Uiso 0.50 1 d P . . O7 O 0.4373(5) -0.016(4) 0.4392(5) 0.030(5) Uani 1 1 d U . . H7 H 0.4737 0.0067 0.4833 0.036 Uiso 0.50 1 calc PR . . O8 O 0.3371(6) 0.199(5) 0.5118(4) 0.036(4) Uani 1 1 d U . . H8 H 0.3434 0.4432 0.0545 0.043 Uiso 0.50 1 d P . . O11 O -0.0848(5) 0.241(6) 0.3676(4) 0.079(13) Uani 1 1 d . . . H11 H 0.1413 0.5999 0.1438 0.094 Uiso 0.50 1 d P . . O12 O 0.0601(6) 0.004(4) 0.4637(5) 0.033(5) Uani 1 1 d U . . H12 H 0.0177 0.0056 0.4850 0.040 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 0.0362(17) 0.026(11) 0.0334(19) 0.000(2) 0.0068(14) -0.002(2) K2 0.0354(18) 0.038(12) 0.044(2) 0.005(2) 0.0021(15) -0.006(2) K3 0.0338(16) 0.027(11) 0.0358(18) 0.004(2) 0.0088(16) -0.008(2) P1 0.0280(19) 0.028(12) 0.031(2) 0.008(3) 0.0043(16) 0.006(3) P2 0.0279(19) 0.025(12) 0.030(2) -0.003(3) -0.0004(15) 0.006(3) P3 0.0303(18) 0.009(12) 0.030(2) -0.004(3) 0.0051(16) -0.008(3) O1 0.052(5) 0.044(13) 0.048(5) -0.005(7) 0.006(4) 0.000(8) O5 0.037(5) 0.037(13) 0.038(4) 0.012(6) 0.009(4) -0.015(7) O9 0.039(4) 0.041(13) 0.048(5) -0.008(7) 0.003(4) -0.010(7) O2 0.033(4) 0.039(13) 0.035(4) 0.007(6) 0.013(3) -0.005(6) O6 0.026(5) 0.05(6) 0.037(6) 0.000(9) 0.005(4) 0.028(9) O10 0.041(5) 0.041(13) 0.042(5) -0.019(7) 0.006(4) 0.002(7) O3 0.047(4) 0.037(13) 0.033(4) 0.009(6) 0.008(4) -0.006(7) O4 0.051(5) 0.047(13) 0.034(4) -0.003(7) 0.024(4) -0.008(7) O7 0.028(4) 0.023(13) 0.031(4) -0.020(5) -0.003(3) 0.000(6) O8 0.044(4) 0.035(13) 0.024(4) -0.016(6) 0.003(3) -0.001(7) O11 0.033(4) 0.18(4) 0.023(5) -0.017(8) 0.009(3) -0.003(10) O12 0.027(4) 0.033(13) 0.041(5) -0.004(6) 0.013(4) -0.003(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 K1 O9 2.819(15) . ? K1 O10 2.720(13) . ? K1 O6 2.719(14) . ? K1 O11 2.720(16) 2_545 ? K1 O2 2.784(13) . ? K1 O5 2.784(12) . ? K1 O4 2.950(16) 1_545 ? K1 O10 2.889(15) 2 ? K1 P2 3.348(4) . ? K1 P3 3.396(5) . ? K1 P3 3.655(7) 2_545 ? K1 P1 3.760(7) . ? K2 O12 2.721(16) 4 ? K2 O8 2.780(15) 4_565 ? K2 O11 2.896(11) 2_545 ? K2 O3 2.897(15) 1_545 ? K2 O12 2.937(17) 4_565 ? K2 O5 2.994(14) 4 ? K2 O2 3.035(15) . ? K2 O9 2.856(11) 4_565 ? K2 P3 3.499(7) 4_565 ? K2 P1 3.650(7) 1_545 ? K2 P2 3.758(7) 4_565 ? K2 K2 4.449(5) 1_545 ? K3 O3 2.670(17) 1_545 ? K3 O7 2.740(16) 2_655 ? K3 O1 2.846(15) . ? K3 O1 2.756(13) 2_645 ? K3 O4 2.858(14) 2_645 ? K3 O6 2.850(13) 2_645 ? K3 O7 2.935(17) 2_645 ? K3 O8 3.031(13) 4_565 ? K3 P1 3.407(4) 2_645 ? K3 P2 3.516(8) 2_645 ? K3 P1 3.746(7) 1_545 ? K3 P1 3.766(8) . ? P1 O4 1.51(2) . ? P1 O2 1.524(11) . ? P1 O3 1.542(12) . ? P1 O1 1.46(2) . ? P1 K3 3.407(4) 2_655 ? P1 K2 3.650(7) 1_565 ? P1 K3 3.746(7) 1_565 ? P2 O6 1.49(2) . ? P2 O5 1.45(2) . ? P2 O7 1.511(9) . ? P2 O8 1.498(11) . ? P2 K3 3.516(8) 2_655 ? P2 K2 3.758(7) 4_566 ? P2 K3 3.853(7) 2_645 ? P3 O9 1.49(2) . ? P3 O10 1.495(19) . ? P3 O11 1.522(13) . ? P3 O12 1.516(10) . ? P3 K2 3.499(7) 4_566 ? P3 K1 3.655(7) 2 ? O1 K3 2.756(13) 2_655 ? O5 K2 2.994(14) 4_556 ? O9 O10 2.38(3) . ? O9 K2 2.856(11) 4_566 ? O6 K3 2.850(13) 2_655 ? O10 K1 2.889(15) 2_545 ? O3 K3 2.670(17) 1_565 ? O3 K2 2.897(15) 1_565 ? O4 K3 2.858(14) 2_655 ? O4 K1 2.950(15) 1_565 ? O7 K3 2.740(16) 2_645 ? O7 K3 2.935(17) 2_655 ? O8 K2 2.780(15) 4_566 ? O8 K3 3.031(13) 4_566 ? O11 K1 2.720(15) 2 ? O11 K2 2.896(11) 2 ? O12 K2 2.721(16) 4_556 ? O12 K2 2.937(17) 4_566 ? 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 O9 K1 O10 50.8(6) . . ? O9 K1 O6 70.8(3) . . ? O10 K1 O6 110.7(3) . . ? O9 K1 O11 136.3(3) . 2_545 ? O10 K1 O11 92.9(4) . 2_545 ? O6 K1 O11 152.9(3) . 2_545 ? O9 K1 O2 120.6(6) . . ? O10 K1 O2 151.5(4) . . ? O6 K1 O2 86.2(4) . . ? O11 K1 O2 78.1(5) 2_545 . ? O9 K1 O5 70.7(5) . . ? O10 K1 O5 74.9(3) . . ? O6 K1 O5 50.9(8) . . ? O11 K1 O5 129.0(8) 2_545 . ? O2 K1 O5 131.5(3) . . ? O9 K1 O4 143.9(3) . 1_545 ? O10 K1 O4 132.6(7) . 1_545 ? O6 K1 O4 77.1(4) . 1_545 ? O11 K1 O4 77.0(4) 2_545 1_545 ? O2 K1 O4 72.2(5) . 1_545 ? O5 K1 O4 76.4(4) . 1_545 ? O9 K1 O10 72.7(4) . 2 ? O10 K1 O10 74.0(3) . 2 ? O6 K1 O10 124.0(7) . 2 ? O11 K1 O10 74.2(5) 2_545 2 ? O2 K1 O10 77.5(4) . 2 ? O5 K1 O10 141.8(4) . 2 ? O4 K1 O10 141.7(3) 1_545 2 ? O9 K1 P2 71.7(2) . . ? O10 K1 P2 94.9(2) . . ? O6 K1 P2 25.9(5) . . ? O11 K1 P2 144.4(4) 2_545 . ? O2 K1 P2 108.1(2) . . ? O5 K1 P2 25.3(4) . . ? O4 K1 P2 72.2(2) 1_545 . ? O10 K1 P2 141.1(4) 2 . ? O9 K1 P3 25.7(5) . . ? O10 K1 P3 25.4(5) . . ? O6 K1 P3 89.5(2) . . ? O11 K1 P3 116.4(2) 2_545 . ? O2 K1 P3 142.0(4) . . ? O5 K1 P3 68.6(3) . . ? O4 K1 P3 143.0(4) 1_545 . ? O10 K1 P3 73.8(2) 2 . ? P2 K1 P3 80.76(11) . . ? O9 K1 P3 115.3(3) . 2_545 ? O10 K1 P3 71.4(3) . 2_545 ? O6 K1 P3 171.0(5) . 2_545 ? O11 K1 P3 21.94(19) 2_545 2_545 ? O2 K1 P3 95.6(3) . 2_545 ? O5 K1 P3 123.5(6) . 2_545 ? O4 K1 P3 94.9(4) 1_545 2_545 ? O10 K1 P3 65.0(5) 2 2_545 ? P2 K1 P3 147.3(3) . 2_545 ? P3 K1 P3 94.46(13) . 2_545 ? O9 K1 P1 116.5(5) . . ? O10 K1 P1 164.8(6) . . ? O6 K1 P1 66.7(3) . . ? O11 K1 P1 93.9(3) 2_545 . ? O2 K1 P1 20.84(18) . . ? O5 K1 P1 110.7(3) . . ? O4 K1 P1 62.3(5) 1_545 . ? O10 K1 P1 94.8(4) 2 . ? P2 K1 P1 87.38(14) . . ? P3 K1 P1 142.1(3) . . ? P3 K1 P1 113.70(12) 2_545 . ? O12 K2 O8 143.4(4) 4 4_565 ? O12 K2 O11 69.1(4) 4 2_545 ? O8 K2 O11 144.5(3) 4_565 2_545 ? O12 K2 O3 101.2(6) 4 1_545 ? O8 K2 O3 74.8(5) 4_565 1_545 ? O11 K2 O3 86.6(4) 2_545 1_545 ? O12 K2 O12 103.6(3) 4 4_565 ? O8 K2 O12 86.0(5) 4_565 4_565 ? O11 K2 O12 101.0(4) 2_545 4_565 ? O3 K2 O12 155.2(6) 1_545 4_565 ? O12 K2 O5 71.0(5) 4 4 ? O8 K2 O5 72.9(6) 4_565 4 ? O11 K2 O5 131.5(8) 2_545 4 ? O3 K2 O5 75.2(4) 1_545 4 ? O12 K2 O5 114.3(4) 4_565 4 ? O12 K2 O2 139.8(3) 4 . ? O8 K2 O2 76.7(4) 4_565 . ? O11 K2 O2 71.5(5) 2_545 . ? O3 K2 O2 84.5(5) 1_545 . ? O12 K2 O2 75.8(4) 4_565 . ? O5 K2 O2 146.9(3) 4 . ? O12 K2 O9 76.1(5) 4 4_565 ? O8 K2 O9 85.1(4) 4_565 4_565 ? O11 K2 O9 125.6(3) 2_545 4_565 ? O3 K2 O9 141.6(4) 1_545 4_565 ? O12 K2 O9 48.7(5) 4_565 4_565 ? O5 K2 O9 67.7(5) 4 4_565 ? O2 K2 O9 122.7(6) . 4_565 ? O12 K2 P3 84.9(3) 4 4_565 ? O8 K2 P3 90.9(4) 4_565 4_565 ? O11 K2 P3 110.3(3) 2_545 4_565 ? O3 K2 P3 163.1(2) 1_545 4_565 ? O12 K2 P3 25.4(2) 4_565 4_565 ? O5 K2 P3 92.2(4) 4 4_565 ? O2 K2 P3 101.2(4) . 4_565 ? O9 K2 P3 24.6(4) 4_565 4_565 ? O12 K2 P1 92.9(3) 4 1_545 ? O8 K2 P1 94.8(3) 4_565 1_545 ? O11 K2 P1 62.7(3) 2_545 1_545 ? O3 K2 P1 23.9(2) 1_545 1_545 ? O12 K2 P1 151.1(3) 4_565 1_545 ? O5 K2 P1 93.3(4) 4 1_545 ? O2 K2 P1 76.3(3) . 1_545 ? O9 K2 P1 160.2(5) 4_565 1_545 ? P3 K2 P1 173.03(13) 4_565 1_545 ? O12 K2 P2 128.3(2) 4 4_565 ? O8 K2 P2 20.23(17) 4_565 4_565 ? O11 K2 P2 162.5(4) 2_545 4_565 ? O3 K2 P2 90.1(3) 1_545 4_565 ? O12 K2 P2 75.5(3) 4_565 4_565 ? O5 K2 P2 63.6(5) 4 4_565 ? O2 K2 P2 91.1(3) . 4_565 ? O9 K2 P2 65.1(3) 4_565 4_565 ? P3 K2 P2 73.95(14) 4_565 4_565 ? P1 K2 P2 112.40(13) 1_545 4_565 ? O12 K2 K2 39.9(3) 4 1_545 ? O8 K2 K2 122.5(5) 4_565 1_545 ? O11 K2 K2 69.9(5) 2_545 1_545 ? O3 K2 K2 61.3(5) 1_545 1_545 ? O12 K2 K2 143.5(3) 4_565 1_545 ? O5 K2 K2 61.9(5) 4 1_545 ? O2 K2 K2 128.9(3) . 1_545 ? O9 K2 K2 106.8(5) 4_565 1_545 ? P3 K2 K2 122.83(16) 4_565 1_545 ? P1 K2 K2 56.82(16) 1_545 1_545 ? P2 K2 K2 122.95(15) 4_565 1_545 ? O3 K3 O7 140.1(4) 1_545 2_655 ? O3 K3 O1 74.6(6) 1_545 . ? O7 K3 O1 104.4(6) 2_655 . ? O3 K3 O1 91.5(5) 1_545 2_645 ? O7 K3 O1 127.9(5) 2_655 2_645 ? O1 K3 O1 78.8(2) . 2_645 ? O3 K3 O4 138.8(4) 1_545 2_645 ? O7 K3 O4 78.0(5) 2_655 2_645 ? O1 K3 O4 81.5(4) . 2_645 ? O1 K3 O4 50.6(7) 2_645 2_645 ? O3 K3 O6 124.6(7) 1_545 2_645 ? O7 K3 O6 77.3(5) 2_655 2_645 ? O1 K3 O6 148.2(3) . 2_645 ? O1 K3 O6 75.8(3) 2_645 2_645 ? O4 K3 O6 67.6(4) 2_645 2_645 ? O3 K3 O7 78.8(5) 1_545 2_645 ? O7 K3 O7 103.2(3) 2_655 2_645 ? O1 K3 O7 151.1(6) . 2_645 ? O1 K3 O7 90.8(6) 2_645 2_645 ? O4 K3 O7 112.6(5) 2_645 2_645 ? O6 K3 O7 48.4(5) 2_645 2_645 ? O3 K3 O8 74.2(5) 1_545 4_565 ? O7 K3 O8 67.0(4) 2_655 4_565 ? O1 K3 O8 77.5(4) . 4_565 ? O1 K3 O8 154.8(3) 2_645 4_565 ? O4 K3 O8 132.5(8) 2_645 4_565 ? O6 K3 O8 129.4(3) 2_645 4_565 ? O7 K3 O8 106.1(4) 2_645 4_565 ? O3 K3 P1 114.4(3) 1_545 2_645 ? O7 K3 P1 104.0(2) 2_655 2_645 ? O1 K3 P1 77.9(2) . 2_645 ? O1 K3 P1 24.6(5) 2_645 2_645 ? O4 K3 P1 26.1(5) 2_645 2_645 ? O6 K3 P1 71.1(2) 2_645 2_645 ? O7 K3 P1 103.5(2) 2_645 2_645 ? O8 K3 P1 150.4(4) 4_565 2_645 ? O3 K3 P2 103.7(5) 1_545 2_645 ? O7 K3 P2 85.9(3) 2_655 2_645 ? O1 K3 P2 166.0(4) . 2_645 ? O1 K3 P2 87.4(4) 2_645 2_645 ? O4 K3 P2 91.6(4) 2_645 2_645 ? O6 K3 P2 24.3(4) 2_645 2_645 ? O7 K3 P2 25.1(2) 2_645 2_645 ? O8 K3 P2 115.8(3) 4_565 2_645 ? P1 K3 P2 90.54(14) 2_645 2_645 ? O3 K3 P1 20.11(17) 1_545 1_545 ? O7 K3 P1 155.4(2) 2_655 1_545 ? O1 K3 P1 63.8(5) . 1_545 ? O1 K3 P1 73.1(4) 2_645 1_545 ? O4 K3 P1 118.7(3) 2_645 1_545 ? O6 K3 P1 124.6(5) 2_645 1_545 ? O7 K3 P1 87.4(3) 2_645 1_545 ? O8 K3 P1 88.8(3) 4_565 1_545 ? P1 K3 P1 94.79(14) 2_645 1_545 ? P2 K3 P1 110.1(2) 2_645 1_545 ? O3 K3 P1 77.0(4) 1_545 . ? O7 K3 P1 89.9(4) 2_655 . ? O1 K3 P1 19.9(4) . . ? O1 K3 P1 98.4(4) 2_645 . ? O4 K3 P1 91.5(4) 2_645 . ? O6 K3 P1 157.3(5) 2_645 . ? O7 K3 P1 154.3(2) 2_645 . ? O8 K3 P1 58.7(3) 4_565 . ? P1 K3 P1 94.43(16) 2_645 . ? P2 K3 P1 174.15(15) 2_645 . ? P1 K3 P1 72.62(10) 1_545 . ? O4 P1 O2 107.9(7) . . ? O4 P1 O3 109.7(11) . . ? O2 P1 O3 110.3(5) . . ? O4 P1 O1 107.9(9) . . ? O2 P1 O1 111.8(12) . . ? O3 P1 O1 109.2(8) . . ? O4 P1 K3 56.2(6) . 2_655 ? O2 P1 K3 128.7(4) . 2_655 ? O3 P1 K3 121.0(4) . 2_655 ? O1 P1 K3 51.9(7) . 2_655 ? O4 P1 K2 94.8(8) . 1_565 ? O2 P1 K2 71.1(5) . 1_565 ? O3 P1 K2 49.5(5) . 1_565 ? O1 P1 K2 154.1(5) . 1_565 ? K3 P1 K2 147.1(3) 2_655 1_565 ? O4 P1 K1 90.5(7) . . ? O2 P1 K1 40.5(4) . . ? O3 P1 K1 150.1(5) . . ? O1 P1 K1 83.8(7) . . ? K3 P1 K1 88.45(14) 2_655 . ? K2 P1 K1 108.77(13) 1_565 . ? O4 P1 K3 83.2(7) . 1_565 ? O2 P1 K3 144.8(5) . 1_565 ? O3 P1 K3 36.5(5) . 1_565 ? O1 P1 K3 95.2(7) . 1_565 ? K3 P1 K3 85.54(14) 2_655 1_565 ? K2 P1 K3 74.88(15) 1_565 1_565 ? K1 P1 K3 173.01(17) . 1_565 ? O4 P1 K3 136.1(4) . . ? O2 P1 K3 113.0(7) . . ? O3 P1 K3 70.3(8) . . ? O1 P1 K3 41.6(4) . . ? K3 P1 K3 85.23(13) 2_655 . ? K2 P1 K3 112.77(14) 1_565 . ? K1 P1 K3 110.5(3) . . ? K3 P1 K3 72.62(10) 1_565 . ? O6 P2 O5 106.8(10) . . ? O6 P2 O7 104.6(7) . . ? O5 P2 O7 118.7(12) . . ? O6 P2 O8 109.7(12) . . ? O5 P2 O8 108.5(8) . . ? O7 P2 O8 108.2(6) . . ? O6 P2 K1 52.8(7) . . ? O5 P2 K1 55.1(6) . . ? O7 P2 K1 118.9(4) . . ? O8 P2 K1 132.3(5) . . ? O6 P2 K3 51.9(4) . 2_655 ? O5 P2 K3 142.9(4) . 2_655 ? O7 P2 K3 55.4(7) . 2_655 ? O8 P2 K3 107.6(8) . 2_655 ? K1 P2 K3 93.61(14) . 2_655 ? O6 P2 K2 82.8(6) . 4_566 ? O5 P2 K2 89.8(8) . 4_566 ? O7 P2 K2 145.6(5) . 4_566 ? O8 P2 K2 39.9(5) . 4_566 ? K1 P2 K2 92.56(13) . 4_566 ? K3 P2 K2 113.2(3) 2_655 4_566 ? O6 P2 K3 106.1(6) . 2_645 ? O5 P2 K3 86.5(8) . 2_645 ? O7 P2 K3 34.2(6) . 2_645 ? O8 P2 K3 134.4(6) . 2_645 ? K1 P2 K3 91.95(15) . 2_645 ? K3 P2 K3 74.11(11) 2_655 2_645 ? K2 P2 K3 171.1(2) 4_566 2_645 ? O9 P3 O10 105.6(9) . . ? O9 P3 O11 109.0(13) . . ? O10 P3 O11 111.1(7) . . ? O9 P3 O12 105.2(7) . . ? O10 P3 O12 114.4(10) . . ? O11 P3 O12 111.1(5) . . ? O9 P3 K1 55.0(7) . . ? O10 P3 K1 51.2(6) . . ? O11 P3 K1 131.1(4) . . ? O12 P3 K1 117.7(4) . . ? O9 P3 K2 52.8(4) . 4_566 ? O10 P3 K2 140.6(4) . 4_566 ? O11 P3 K2 107.4(7) . 4_566 ? O12 P3 K2 56.1(7) . 4_566 ? K1 P3 K2 96.50(13) . 4_566 ? O9 P3 K1 80.9(6) . 2 ? O10 P3 K1 90.5(6) . 2 ? O11 P3 K1 41.9(5) . 2 ? O12 P3 K1 150.8(6) . 2 ? K1 P3 K1 89.54(14) . 2 ? K2 P3 K1 113.8(3) 4_566 2 ? P1 O1 K3 118.5(5) . . ? P1 O1 K3 103.6(11) . 2_655 ? K3 O1 K3 120.5(3) . 2_655 ? P2 O5 K1 99.6(9) . . ? P2 O5 K2 122.3(5) . 4_556 ? K1 O5 K2 130.1(3) . 4_556 ? P3 O9 O10 37.2(6) . . ? P3 O9 K1 99.3(11) . . ? O10 O9 K1 62.4(5) . . ? P3 O9 K2 102.6(5) . 4_566 ? O10 O9 K2 130.0(8) . 4_566 ? K1 O9 K2 130.0(4) . 4_566 ? P1 O2 K1 118.6(5) . . ? P1 O2 K2 114.3(6) . . ? K1 O2 K2 101.2(6) . . ? P2 O6 K1 101.3(12) . . ? P2 O6 K3 103.7(4) . 2_655 ? K1 O6 K3 128.0(3) . 2_655 ? P3 O10 O9 37.1(6) . . ? P3 O10 K1 103.5(10) . . ? O9 O10 K1 66.7(6) . . ? P3 O10 K1 122.9(5) . 2_545 ? O9 O10 K1 145.2(8) . 2_545 ? K1 O10 K1 124.7(3) . 2_545 ? P1 O3 K3 123.4(6) . 1_565 ? P1 O3 K2 106.6(5) . 1_565 ? K3 O3 K2 107.7(8) 1_565 1_565 ? P1 O4 K3 97.7(10) . 2_655 ? P1 O4 K1 123.1(5) . 1_565 ? K3 O4 K1 126.7(3) 2_655 1_565 ? P2 O7 K3 127.7(8) . 2_645 ? P2 O7 K3 99.5(8) . 2_655 ? K3 O7 K3 103.2(3) 2_645 2_655 ? P2 O8 K2 119.8(5) . 4_566 ? P2 O8 K3 128.7(5) . 4_566 ? K2 O8 K3 101.3(6) 4_566 4_566 ? P3 O11 K1 116.2(5) . 2 ? P3 O11 K2 130.9(4) . 2 ? K1 O11 K2 106.5(6) 2 2 ? P3 O12 K2 131.4(8) . 4_556 ? P3 O12 K2 98.5(8) . 4_566 ? K2 O12 K2 103.6(3) 4_556 4_566 ? _diffrn_measured_fraction_theta_max 0.190 _diffrn_reflns_theta_full 26.51 _diffrn_measured_fraction_theta_full 0.190 _refine_diff_density_max 0.519 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.107 #===END data_KDP_1.68GPa CSD-424770 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Andrzej Katrusiak' _publ_contact_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_fax '+48(61)8291505' _publ_contact_author_phone '+48(61)8291443' _publ_contact_author_email katran@amu.edu.pl _publ_section_title ; ? ; loop_ _publ_author_footnote ; Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _chemical_name_systematic ; ? ; _chemical_name_common PotassiumDihydrogenPhosphate _chemical_melting_point ? _chemical_formula_moiety 'H2 O4 P, K' _chemical_formula_sum 'H2 K O4 P' _chemical_formula_weight 136.09 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I -4 2bw ' 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' _cell_length_a 7.345(5) _cell_length_b 7.345(5) _cell_length_c 6.8756(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 371.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_pressure 1680000 _cell_measurement_reflns_used 848 _cell_measurement_theta_min 4.06 _cell_measurement_theta_max 27.88 _exptl_crystal_description 'plate-shaped' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 272 _exptl_absorpt_coefficient_mu 1.716 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.2843 _exptl_absorpt_correction_T_max 0.6183 _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_special_details ; Data were collected at room temperature and pressure of 1.68(3) GPa (1680000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 848 _diffrn_reflns_av_R_equivalents 0.1192 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.06 _diffrn_reflns_theta_max 27.88 _reflns_number_total 52 _reflns_number_gt 51 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+0.2831P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.03(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(4) _refine_ls_number_reflns 52 _refine_ls_number_parameters 16 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 K1 K 0.0000 0.0000 0.5000 0.0238(11) Uani 1 4 d S . . P1 P 0.0000 0.0000 0.0000 0.0203(11) Uani 1 4 d S . . O1 O 0.1518(3) 0.0807(6) 0.1272(4) 0.0245(12) Uani 1 1 d . . . H1 H 0.1518 0.1919 0.1165 0.05(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 0.0248(13) 0.0248(13) 0.0217(13) 0.000 0.000 0.000 P1 0.0196(14) 0.0196(14) 0.0217(14) 0.000 0.000 0.000 O1 0.0220(18) 0.025(2) 0.0266(14) -0.0022(13) -0.005(3) 0.006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 K1 O1 2.758(3) 5 ? K1 O1 2.758(3) 16_444 ? K1 O1 2.758(3) 6_455 ? K1 O1 2.758(3) 15_454 ? K1 O1 2.858(3) 2 ? K1 O1 2.858(3) 4_556 ? K1 O1 2.858(3) 3_556 ? K1 O1 2.858(3) . ? K1 P1 3.4378(8) . ? K1 P1 3.4378(8) 1_556 ? K1 K1 4.055(2) 5_455 ? K1 K1 4.055(2) 13_455 ? P1 O1 1.536(3) . ? P1 O1 1.536(3) 2 ? P1 O1 1.536(3) 3 ? P1 O1 1.536(3) 4 ? P1 K1 3.4378(8) 1_554 ? O1 K1 2.758(3) 5 ? 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 K1 O1 95.38(4) 5 16_444 ? O1 K1 O1 144.34(13) 5 6_455 ? O1 K1 O1 95.38(4) 16_444 6_455 ? O1 K1 O1 95.38(4) 5 15_454 ? O1 K1 O1 144.34(13) 16_444 15_454 ? O1 K1 O1 95.38(4) 6_455 15_454 ? O1 K1 O1 132.94(7) 5 2 ? O1 K1 O1 67.47(6) 16_444 2 ? O1 K1 O1 82.42(9) 6_455 2 ? O1 K1 O1 80.44(9) 15_454 2 ? O1 K1 O1 80.44(9) 5 4_556 ? O1 K1 O1 132.94(7) 16_444 4_556 ? O1 K1 O1 67.47(6) 6_455 4_556 ? O1 K1 O1 82.42(9) 15_454 4_556 ? O1 K1 O1 143.57(7) 2 4_556 ? O1 K1 O1 67.47(6) 5 3_556 ? O1 K1 O1 82.42(9) 16_444 3_556 ? O1 K1 O1 80.44(9) 6_455 3_556 ? O1 K1 O1 132.94(7) 15_454 3_556 ? O1 K1 O1 143.57(7) 2 3_556 ? O1 K1 O1 52.46(10) 4_556 3_556 ? O1 K1 O1 82.42(9) 5 . ? O1 K1 O1 80.44(9) 16_444 . ? O1 K1 O1 132.94(7) 6_455 . ? O1 K1 O1 67.47(6) 15_454 . ? O1 K1 O1 52.46(10) 2 . ? O1 K1 O1 143.57(7) 4_556 . ? O1 K1 O1 143.57(7) 3_556 . ? O1 K1 P1 107.83(7) 5 . ? O1 K1 P1 72.17(7) 16_444 . ? O1 K1 P1 107.83(7) 6_455 . ? O1 K1 P1 72.17(7) 15_454 . ? O1 K1 P1 26.23(5) 2 . ? O1 K1 P1 153.77(5) 4_556 . ? O1 K1 P1 153.77(5) 3_556 . ? O1 K1 P1 26.23(5) . . ? O1 K1 P1 72.17(7) 5 1_556 ? O1 K1 P1 107.83(7) 16_444 1_556 ? O1 K1 P1 72.17(7) 6_455 1_556 ? O1 K1 P1 107.83(7) 15_454 1_556 ? O1 K1 P1 153.77(5) 2 1_556 ? O1 K1 P1 26.23(5) 4_556 1_556 ? O1 K1 P1 26.23(5) 3_556 1_556 ? O1 K1 P1 153.77(5) . 1_556 ? P1 K1 P1 180.0 . 1_556 ? O1 K1 K1 165.86(8) 5 5_455 ? O1 K1 K1 93.73(8) 16_444 5_455 ? O1 K1 K1 44.76(7) 6_455 5_455 ? O1 K1 K1 71.06(8) 15_454 5_455 ? O1 K1 K1 42.80(5) 2 5_455 ? O1 K1 K1 101.09(8) 4_556 5_455 ? O1 K1 K1 124.63(8) 3_556 5_455 ? O1 K1 K1 88.47(5) . 5_455 ? P1 K1 K1 64.919(14) . 5_455 ? P1 K1 K1 115.081(14) 1_556 5_455 ? O1 K1 K1 71.06(8) 5 13_455 ? O1 K1 K1 165.86(8) 16_444 13_455 ? O1 K1 K1 93.73(8) 6_455 13_455 ? O1 K1 K1 44.76(7) 15_454 13_455 ? O1 K1 K1 124.63(8) 2 13_455 ? O1 K1 K1 42.80(5) 4_556 13_455 ? O1 K1 K1 88.47(5) 3_556 13_455 ? O1 K1 K1 101.09(8) . 13_455 ? P1 K1 K1 115.081(14) . 13_455 ? P1 K1 K1 64.919(14) 1_556 13_455 ? K1 K1 K1 100.352(11) 5_455 13_455 ? O1 P1 O1 110.6(2) . 2 ? O1 P1 O1 108.91(11) . 3 ? O1 P1 O1 108.91(11) 2 3 ? O1 P1 O1 108.91(11) . 4 ? O1 P1 O1 108.91(11) 2 4 ? O1 P1 O1 110.6(2) 3 4 ? O1 P1 K1 124.70(11) . 1_554 ? O1 P1 K1 124.70(11) 2 1_554 ? O1 P1 K1 55.30(11) 3 1_554 ? O1 P1 K1 55.30(11) 4 1_554 ? O1 P1 K1 55.30(11) . . ? O1 P1 K1 55.30(11) 2 . ? O1 P1 K1 124.70(11) 3 . ? O1 P1 K1 124.70(11) 4 . ? K1 P1 K1 180.0 1_554 . ? P1 O1 K1 139.9(2) . 5 ? P1 O1 K1 98.46(13) . . ? K1 O1 K1 92.44(9) 5 . ? _diffrn_measured_fraction_theta_max 0.374 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.374 _refine_diff_density_max 0.246 _refine_diff_density_min -0.162 _refine_diff_density_rms 0.062 #===END data_KDP_1.76GPa CSD-424771 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Andrzej Katrusiak' _publ_contact_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_fax '+48(61)8291505' _publ_contact_author_phone '+48(61)8291443' _publ_contact_author_email katran@amu.edu.pl _publ_section_title ; ? ; loop_ _publ_author_footnote ; Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _chemical_name_systematic ; ? ; _chemical_name_common PotassiumDihydrogenPhosphate _chemical_melting_point ? _chemical_formula_moiety 'H2 O4 P, K' _chemical_formula_sum 'H2 K O4 P' _chemical_formula_weight 136.09 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I -4 2bw ' 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' _cell_length_a 7.340(7) _cell_length_b 7.340(7) _cell_length_c 6.865(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 369.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_pressure 1760000 _cell_measurement_reflns_used 558 _cell_measurement_theta_min 4.06 _cell_measurement_theta_max 27.55 _exptl_crystal_description 'plate-shaped' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 272 _exptl_absorpt_coefficient_mu 1.721 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.2849 _exptl_absorpt_correction_T_max 0.6352 _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_special_details ; Data were collected at room temperature and pressure of 1.76(3) GPa (1760000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _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_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 558 _diffrn_reflns_av_R_equivalents 0.2944 _diffrn_reflns_av_sigmaI/netI 0.0896 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.06 _diffrn_reflns_theta_max 27.55 _reflns_number_total 44 _reflns_number_gt 43 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(3) _refine_ls_number_reflns 44 _refine_ls_number_parameters 15 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0459 _refine_ls_wR_factor_gt 0.0456 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 K1 K 0.0000 0.0000 0.5000 0.0379(9) Uani 1 4 d S . . P1 P 0.0000 0.0000 0.0000 0.0325(10) Uani 1 4 d S . . O1 O 0.1503(3) 0.0807(5) 0.1261(4) 0.0404(9) Uani 1 1 d . . . H1 H 0.1499 0.1919 0.1153 0.08(6) 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 0.0405(13) 0.0405(13) 0.0326(12) 0.000 0.000 0.000 P1 0.0316(14) 0.0316(14) 0.0344(14) 0.000 0.000 0.000 O1 0.0457(16) 0.039(2) 0.0370(12) -0.0118(15) 0.002(3) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 K1 O1 2.768(4) 5 ? K1 O1 2.768(4) 16_444 ? K1 O1 2.768(4) 6_455 ? K1 O1 2.768(4) 15_454 ? K1 O1 2.856(3) 2 ? K1 O1 2.856(3) 4_556 ? K1 O1 2.856(3) 3_556 ? K1 O1 2.856(3) . ? K1 P1 3.4327(17) . ? K1 P1 3.4327(17) 1_556 ? K1 K1 4.051(3) 5_455 ? K1 K1 4.051(3) 13_455 ? P1 O1 1.522(3) . ? P1 O1 1.522(3) 3 ? P1 O1 1.522(3) 4 ? P1 O1 1.522(3) 2 ? P1 K1 3.4327(17) 1_554 ? O1 K1 2.768(4) 5 ? 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 K1 O1 95.42(4) 5 16_444 ? O1 K1 O1 144.21(13) 5 6_455 ? O1 K1 O1 95.42(4) 16_444 6_455 ? O1 K1 O1 95.42(4) 5 15_454 ? O1 K1 O1 144.21(13) 16_444 15_454 ? O1 K1 O1 95.42(4) 6_455 15_454 ? O1 K1 O1 132.74(7) 5 2 ? O1 K1 O1 67.31(6) 16_444 2 ? O1 K1 O1 82.74(10) 6_455 2 ? O1 K1 O1 80.41(9) 15_454 2 ? O1 K1 O1 80.41(9) 5 4_556 ? O1 K1 O1 132.74(7) 16_444 4_556 ? O1 K1 O1 67.31(6) 6_455 4_556 ? O1 K1 O1 82.74(10) 15_454 4_556 ? O1 K1 O1 143.89(7) 2 4_556 ? O1 K1 O1 67.31(6) 5 3_556 ? O1 K1 O1 82.74(10) 16_444 3_556 ? O1 K1 O1 80.41(9) 6_455 3_556 ? O1 K1 O1 132.74(7) 15_454 3_556 ? O1 K1 O1 143.89(7) 2 3_556 ? O1 K1 O1 52.00(11) 4_556 3_556 ? O1 K1 O1 82.74(10) 5 . ? O1 K1 O1 80.41(9) 16_444 . ? O1 K1 O1 132.74(7) 6_455 . ? O1 K1 O1 67.31(6) 15_454 . ? O1 K1 O1 52.00(11) 2 . ? O1 K1 O1 143.89(7) 4_556 . ? O1 K1 O1 143.89(7) 3_556 . ? O1 K1 P1 107.89(7) 5 . ? O1 K1 P1 72.11(7) 16_444 . ? O1 K1 P1 107.89(7) 6_455 . ? O1 K1 P1 72.11(7) 15_454 . ? O1 K1 P1 26.00(5) 2 . ? O1 K1 P1 154.00(5) 4_556 . ? O1 K1 P1 154.00(5) 3_556 . ? O1 K1 P1 26.00(5) . . ? O1 K1 P1 72.11(7) 5 1_556 ? O1 K1 P1 107.89(7) 16_444 1_556 ? O1 K1 P1 72.11(7) 6_455 1_556 ? O1 K1 P1 107.89(7) 15_454 1_556 ? O1 K1 P1 154.00(5) 2 1_556 ? O1 K1 P1 26.00(5) 4_556 1_556 ? O1 K1 P1 26.00(5) 3_556 1_556 ? O1 K1 P1 154.00(5) . 1_556 ? P1 K1 P1 180.0 . 1_556 ? O1 K1 K1 165.96(7) 5 5_455 ? O1 K1 K1 93.64(7) 16_444 5_455 ? O1 K1 K1 44.78(8) 6_455 5_455 ? O1 K1 K1 71.10(7) 15_454 5_455 ? O1 K1 K1 43.06(5) 2 5_455 ? O1 K1 K1 101.13(8) 4_556 5_455 ? O1 K1 K1 124.65(7) 3_556 5_455 ? O1 K1 K1 88.23(7) . 5_455 ? P1 K1 K1 64.94(2) . 5_455 ? P1 K1 K1 115.06(2) 1_556 5_455 ? O1 K1 K1 71.10(7) 5 13_455 ? O1 K1 K1 165.96(7) 16_444 13_455 ? O1 K1 K1 93.64(7) 6_455 13_455 ? O1 K1 K1 44.78(8) 15_454 13_455 ? O1 K1 K1 124.65(7) 2 13_455 ? O1 K1 K1 43.06(5) 4_556 13_455 ? O1 K1 K1 88.23(7) 3_556 13_455 ? O1 K1 K1 101.13(8) . 13_455 ? P1 K1 K1 115.06(2) . 13_455 ? P1 K1 K1 64.94(2) 1_556 13_455 ? K1 K1 K1 100.339(19) 5_455 13_455 ? O1 P1 O1 108.88(12) . 3 ? O1 P1 O1 108.88(12) . 4 ? O1 P1 O1 110.7(2) 3 4 ? O1 P1 O1 110.7(2) . 2 ? O1 P1 O1 108.88(12) 3 2 ? O1 P1 O1 108.88(12) 4 2 ? O1 P1 K1 55.33(12) . . ? O1 P1 K1 124.67(12) 3 . ? O1 P1 K1 124.67(12) 4 . ? O1 P1 K1 55.33(12) 2 . ? O1 P1 K1 124.67(12) . 1_554 ? O1 P1 K1 55.33(12) 3 1_554 ? O1 P1 K1 55.33(12) 4 1_554 ? O1 P1 K1 124.67(12) 2 1_554 ? K1 P1 K1 180.0 . 1_554 ? P1 O1 K1 139.78(19) . 5 ? P1 O1 K1 98.67(13) . . ? K1 O1 K1 92.16(10) 5 . ? _diffrn_measured_fraction_theta_max 0.328 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.328 _refine_diff_density_max 0.151 _refine_diff_density_min -0.174 _refine_diff_density_rms 0.039 #===END data_KDP_1.91GPa CSD-424772 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Andrzej Katrusiak' _publ_contact_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_fax '+48(61)8291505' _publ_contact_author_phone '+48(61)8291443' _publ_contact_author_email katran@amu.edu.pl _publ_section_title ; ? ; loop_ _publ_author_footnote ; Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _chemical_name_systematic ; ? ; _chemical_name_common PotassiumDihydrogenPhosphate _chemical_melting_point ? _chemical_formula_moiety 'H2 O4 P, K' _chemical_formula_sum 'H2 K O4 P' _chemical_formula_weight 136.09 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I -4 2bw ' 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' _cell_length_a 7.330(4) _cell_length_b 7.330(4) _cell_length_c 6.8542(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 368.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_pressure 1910000 _cell_measurement_reflns_used 784 _cell_measurement_theta_min 4.07 _cell_measurement_theta_max 27.98 _exptl_crystal_description 'plate-shaped' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 272 _exptl_absorpt_coefficient_mu 1.728 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.3587 _exptl_absorpt_correction_T_max 0.6879 _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_special_details ; Data were collected at room temperature and pressure of 1.91(3) GPa (1910000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _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_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 784 _diffrn_reflns_av_R_equivalents 0.0805 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 27.98 _reflns_number_total 57 _reflns_number_gt 57 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.6624P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(4) _refine_ls_number_reflns 57 _refine_ls_number_parameters 15 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0725 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.326 _refine_ls_restrained_S_all 1.326 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 K1 K 0.0000 0.0000 0.5000 0.0226(9) Uani 1 4 d S . . P1 P 0.0000 0.0000 0.0000 0.0198(10) Uani 1 4 d S . . O1 O 0.1522(5) 0.0811(6) 0.1273(5) 0.0240(11) Uani 1 1 d . . . H1 H 0.1519 0.1925 0.1166 0.8(8) 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 0.0235(12) 0.0235(12) 0.0207(10) 0.000 0.000 0.000 P1 0.0202(14) 0.0202(14) 0.0190(12) 0.000 0.000 0.000 O1 0.0160(19) 0.028(2) 0.0286(16) -0.0019(19) -0.007(3) 0.000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 K1 O1 2.750(4) 5 ? K1 O1 2.750(4) 16_444 ? K1 O1 2.750(4) 15_454 ? K1 O1 2.750(4) 6_455 ? K1 O1 2.850(4) 2 ? K1 O1 2.850(4) 4_556 ? K1 O1 2.850(4) 3_556 ? K1 O1 2.850(4) . ? K1 P1 3.4271(6) . ? K1 P1 3.4271(6) 1_556 ? K1 K1 4.046(2) 5_455 ? K1 K1 4.046(2) 13_455 ? P1 O1 1.536(3) . ? P1 O1 1.536(3) 2 ? P1 O1 1.536(3) 3 ? P1 O1 1.536(3) 4 ? P1 K1 3.4271(6) 1_554 ? O1 K1 2.750(4) 5 ? 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 K1 O1 95.37(4) 5 16_444 ? O1 K1 O1 95.37(5) 5 15_454 ? O1 K1 O1 144.37(15) 16_444 15_454 ? O1 K1 O1 144.37(15) 5 6_455 ? O1 K1 O1 95.37(4) 16_444 6_455 ? O1 K1 O1 95.37(4) 15_454 6_455 ? O1 K1 O1 133.01(10) 5 2 ? O1 K1 O1 67.48(7) 16_444 2 ? O1 K1 O1 80.48(10) 15_454 2 ? O1 K1 O1 82.31(11) 6_455 2 ? O1 K1 O1 80.48(10) 5 4_556 ? O1 K1 O1 133.01(10) 16_444 4_556 ? O1 K1 O1 82.31(11) 15_454 4_556 ? O1 K1 O1 67.48(7) 6_455 4_556 ? O1 K1 O1 143.45(9) 2 4_556 ? O1 K1 O1 67.48(7) 5 3_556 ? O1 K1 O1 82.31(11) 16_444 3_556 ? O1 K1 O1 133.01(10) 15_454 3_556 ? O1 K1 O1 80.48(10) 6_455 3_556 ? O1 K1 O1 143.45(9) 2 3_556 ? O1 K1 O1 52.65(14) 4_556 3_556 ? O1 K1 O1 82.31(11) 5 . ? O1 K1 O1 80.48(10) 16_444 . ? O1 K1 O1 67.48(7) 15_454 . ? O1 K1 O1 133.01(10) 6_455 . ? O1 K1 O1 52.65(14) 2 . ? O1 K1 O1 143.45(10) 4_556 . ? O1 K1 O1 143.45(9) 3_556 . ? O1 K1 P1 107.82(8) 5 . ? O1 K1 P1 72.18(8) 16_444 . ? O1 K1 P1 72.18(8) 15_454 . ? O1 K1 P1 107.82(8) 6_455 . ? O1 K1 P1 26.33(7) 2 . ? O1 K1 P1 153.67(7) 4_556 . ? O1 K1 P1 153.67(7) 3_556 . ? O1 K1 P1 26.33(7) . . ? O1 K1 P1 72.18(8) 5 1_556 ? O1 K1 P1 107.82(8) 16_444 1_556 ? O1 K1 P1 107.82(8) 15_454 1_556 ? O1 K1 P1 72.18(8) 6_455 1_556 ? O1 K1 P1 153.67(7) 2 1_556 ? O1 K1 P1 26.33(7) 4_556 1_556 ? O1 K1 P1 26.33(7) 3_556 1_556 ? O1 K1 P1 153.67(7) . 1_556 ? P1 K1 P1 180.0 . 1_556 ? O1 K1 K1 165.81(8) 5 5_455 ? O1 K1 K1 93.80(9) 16_444 5_455 ? O1 K1 K1 71.01(9) 15_454 5_455 ? O1 K1 K1 44.74(8) 6_455 5_455 ? O1 K1 K1 42.76(8) 2 5_455 ? O1 K1 K1 100.99(9) 4_556 5_455 ? O1 K1 K1 124.65(9) 3_556 5_455 ? O1 K1 K1 88.56(8) . 5_455 ? P1 K1 K1 64.942(14) . 5_455 ? P1 K1 K1 115.058(14) 1_556 5_455 ? O1 K1 K1 71.01(9) 5 13_455 ? O1 K1 K1 165.81(8) 16_444 13_455 ? O1 K1 K1 44.74(8) 15_454 13_455 ? O1 K1 K1 93.80(9) 6_455 13_455 ? O1 K1 K1 124.65(9) 2 13_455 ? O1 K1 K1 42.76(8) 4_556 13_455 ? O1 K1 K1 88.56(8) 3_556 13_455 ? O1 K1 K1 100.99(9) . 13_455 ? P1 K1 K1 115.058(14) . 13_455 ? P1 K1 K1 64.942(14) 1_556 13_455 ? K1 K1 K1 100.334(11) 5_455 13_455 ? O1 P1 O1 110.8(3) . 2 ? O1 P1 O1 108.82(14) . 3 ? O1 P1 O1 108.82(14) 2 3 ? O1 P1 O1 108.82(14) . 4 ? O1 P1 O1 108.82(14) 2 4 ? O1 P1 O1 110.8(3) 3 4 ? O1 P1 K1 124.61(14) . 1_554 ? O1 P1 K1 124.61(14) 2 1_554 ? O1 P1 K1 55.39(14) 3 1_554 ? O1 P1 K1 55.39(14) 4 1_554 ? O1 P1 K1 55.39(14) . . ? O1 P1 K1 55.39(14) 2 . ? O1 P1 K1 124.61(14) 3 . ? O1 P1 K1 124.61(14) 4 . ? K1 P1 K1 180.0 1_554 . ? P1 O1 K1 139.8(2) . 5 ? P1 O1 K1 98.28(17) . . ? K1 O1 K1 92.50(11) 5 . ? _diffrn_measured_fraction_theta_max 0.404 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.404 _refine_diff_density_max 0.118 _refine_diff_density_min -0.120 _refine_diff_density_rms 0.037 #===END data_KDP_2.28GPa CSD-424773 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Andrzej Katrusiak' _publ_contact_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_fax '+48(61)8291505' _publ_contact_author_phone '+48(61)8291443' _publ_contact_author_email katran@amu.edu.pl _publ_section_title ; ? ; loop_ _publ_author_footnote ; Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_author_address ;Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _chemical_name_systematic ; ? ; _chemical_name_common PotassiumDihydrogenPhosphate _chemical_melting_point ? _chemical_formula_moiety 'H2 O4 P, K' _chemical_formula_sum 'H2 K O4 P' _chemical_formula_weight 136.09 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I -4 2bw ' 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' _cell_length_a 7.305(6) _cell_length_b 7.305(6) _cell_length_c 6.8316(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 364.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_pressure 2280000 _cell_measurement_reflns_used 603 _cell_measurement_theta_min 4.09 _cell_measurement_theta_max 27.61 _exptl_crystal_description 'plate-shaped' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 272 _exptl_absorpt_coefficient_mu 1.746 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.3864 _exptl_absorpt_correction_T_max 0.6860 _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_special_details ; Data were collected at room temperature and pressure of 2.28(3) GPa (2280000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _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_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 603 _diffrn_reflns_av_R_equivalents 0.2294 _diffrn_reflns_av_sigmaI/netI 0.1227 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 27.70 _reflns_number_total 47 _reflns_number_gt 46 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+0.1417P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(3) _refine_ls_number_reflns 47 _refine_ls_number_parameters 15 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.193 _refine_ls_restrained_S_all 1.193 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 K1 K 0.0000 0.0000 0.5000 0.0288(17) Uani 1 4 d S . . P1 P 0.0000 0.0000 0.0000 0.0248(19) Uani 1 4 d S . . O1 O 0.1518(4) 0.0815(6) 0.1292(4) 0.0276(11) Uani 1 1 d . . . H1 H 0.1527 0.1932 0.1172 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 0.030(2) 0.030(2) 0.0256(19) 0.000 0.000 0.000 P1 0.026(3) 0.026(3) 0.023(2) 0.000 0.000 0.000 O1 0.028(2) 0.025(3) 0.0295(14) -0.0009(14) -0.011(2) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 K1 O1 2.739(4) 5 ? K1 O1 2.739(4) 16_444 ? K1 O1 2.739(4) 15_454 ? K1 O1 2.739(4) 6_455 ? K1 O1 2.829(3) 2 ? K1 O1 2.829(3) 4_556 ? K1 O1 2.829(3) 3_556 ? K1 O1 2.829(3) . ? K1 P1 3.4158(9) . ? K1 P1 3.4158(9) 1_556 ? K1 K1 4.032(3) 5_455 ? K1 K1 4.032(3) 13_455 ? P1 O1 1.537(3) . ? P1 O1 1.537(3) 2 ? P1 O1 1.537(3) 4 ? P1 O1 1.537(3) 3 ? P1 K1 3.4158(9) 1_554 ? O1 K1 2.739(4) 5 ? 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 K1 O1 95.21(4) 5 16_444 ? O1 K1 O1 95.21(4) 5 15_454 ? O1 K1 O1 144.93(13) 16_444 15_454 ? O1 K1 O1 144.93(13) 5 6_455 ? O1 K1 O1 95.21(4) 16_444 6_455 ? O1 K1 O1 95.21(4) 15_454 6_455 ? O1 K1 O1 132.81(9) 5 2 ? O1 K1 O1 67.67(6) 16_444 2 ? O1 K1 O1 80.82(10) 15_454 2 ? O1 K1 O1 81.95(8) 6_455 2 ? O1 K1 O1 80.82(10) 5 4_556 ? O1 K1 O1 132.81(9) 16_444 4_556 ? O1 K1 O1 81.95(8) 15_454 4_556 ? O1 K1 O1 67.67(6) 6_455 4_556 ? O1 K1 O1 143.32(7) 2 4_556 ? O1 K1 O1 67.67(6) 5 3_556 ? O1 K1 O1 81.95(8) 16_444 3_556 ? O1 K1 O1 132.81(9) 15_454 3_556 ? O1 K1 O1 80.82(10) 6_455 3_556 ? O1 K1 O1 143.32(7) 2 3_556 ? O1 K1 O1 52.84(11) 4_556 3_556 ? O1 K1 O1 81.95(8) 5 . ? O1 K1 O1 80.82(10) 16_444 . ? O1 K1 O1 67.67(6) 15_454 . ? O1 K1 O1 132.81(9) 6_455 . ? O1 K1 O1 52.84(11) 2 . ? O1 K1 O1 143.32(7) 4_556 . ? O1 K1 O1 143.32(7) 3_556 . ? O1 K1 P1 107.53(6) 5 . ? O1 K1 P1 72.47(6) 16_444 . ? O1 K1 P1 72.47(6) 15_454 . ? O1 K1 P1 107.53(6) 6_455 . ? O1 K1 P1 26.42(6) 2 . ? O1 K1 P1 153.58(6) 4_556 . ? O1 K1 P1 153.58(6) 3_556 . ? O1 K1 P1 26.42(6) . . ? O1 K1 P1 72.47(6) 5 1_556 ? O1 K1 P1 107.53(6) 16_444 1_556 ? O1 K1 P1 107.53(6) 15_454 1_556 ? O1 K1 P1 72.47(6) 6_455 1_556 ? O1 K1 P1 153.58(6) 2 1_556 ? O1 K1 P1 26.42(6) 4_556 1_556 ? O1 K1 P1 26.42(6) 3_556 1_556 ? O1 K1 P1 153.58(6) . 1_556 ? P1 K1 P1 180.0 . 1_556 ? O1 K1 K1 165.61(8) 5 5_455 ? O1 K1 K1 93.97(9) 16_444 5_455 ? O1 K1 K1 71.07(9) 15_454 5_455 ? O1 K1 K1 44.49(7) 6_455 5_455 ? O1 K1 K1 42.74(6) 2 5_455 ? O1 K1 K1 100.88(9) 4_556 5_455 ? O1 K1 K1 124.75(9) 3_556 5_455 ? O1 K1 K1 88.61(6) . 5_455 ? P1 K1 K1 64.939(19) . 5_455 ? P1 K1 K1 115.061(19) 1_556 5_455 ? O1 K1 K1 71.07(9) 5 13_455 ? O1 K1 K1 165.61(8) 16_444 13_455 ? O1 K1 K1 44.49(7) 15_454 13_455 ? O1 K1 K1 93.97(9) 6_455 13_455 ? O1 K1 K1 124.75(9) 2 13_455 ? O1 K1 K1 42.74(6) 4_556 13_455 ? O1 K1 K1 88.61(6) 3_556 13_455 ? O1 K1 K1 100.88(9) . 13_455 ? P1 K1 K1 115.061(19) . 13_455 ? P1 K1 K1 64.939(19) 1_556 13_455 ? K1 K1 K1 100.336(15) 5_455 13_455 ? O1 P1 O1 109.9(2) . 2 ? O1 P1 O1 109.25(12) . 4 ? O1 P1 O1 109.25(12) 2 4 ? O1 P1 O1 109.25(12) . 3 ? O1 P1 O1 109.25(12) 2 3 ? O1 P1 O1 109.9(2) 4 3 ? O1 P1 K1 125.04(12) . 1_554 ? O1 P1 K1 125.04(12) 2 1_554 ? O1 P1 K1 54.96(12) 4 1_554 ? O1 P1 K1 54.96(12) 3 1_554 ? O1 P1 K1 54.96(12) . . ? O1 P1 K1 54.96(12) 2 . ? O1 P1 K1 125.04(12) 4 . ? O1 P1 K1 125.04(12) 3 . ? K1 P1 K1 180.0 1_554 . ? P1 O1 K1 139.3(2) . 5 ? P1 O1 K1 98.62(15) . . ? K1 O1 K1 92.78(9) 5 . ? _diffrn_measured_fraction_theta_max 0.351 _diffrn_reflns_theta_full 27.70 _diffrn_measured_fraction_theta_full 0.351 _refine_diff_density_max 0.103 _refine_diff_density_min -0.090 _refine_diff_density_rms 0.033