#------------------------------------------------------------------------------ #$Date: 2025-06-02 16:27:15 +0100 (Mon, 02 Jun 2025) $ #$Revision: 299903 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/01/3500142.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_3500142 loop_ _publ_author_name 'Thierry Maris' _publ_section_references ; APEX4 (2022) Bruker AXS Inc. Madison, WI 53719-1173 Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. SADABS-2016/2 Bruker AXS Inc. Madison, WI 53719-1173 SAINT (2020) V8.40B, Integration for Single Crystal Data. Bruker AXS Inc. Madison, WI 53719-1173 Sheldrick, G.M. (2015a). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015b). Acta Cryst. C71, 3-8. ; _publ_section_title ; Potassium Dihydrogen Phosphate - Monoclinic Form at 150 K / Ambient Pressure ; _journal_name_full 'Personal communication to COD' _journal_year 2025 _chemical_formula_moiety 'H2 O4 P, K' _chemical_formula_sum 'H2 K O4 P' _chemical_formula_weight 136.09 _chemical_name_common 'Potassium Dihydrogen Phosphate' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _audit_creation_date 2025-06-02 _audit_creation_method ; Olex2 1.5 (compiled 2025.05.22 svn.r631f81ec for OlexSys, GUI svn.r7248) ; _cell_angle_alpha 90 _cell_angle_beta 108.015(4) _cell_angle_gamma 90 _cell_formula_units_Z 12 _cell_length_a 14.6427(13) _cell_length_b 4.5086(4) _cell_length_c 18.7214(17) _cell_measurement_reflns_used 9888 _cell_measurement_temperature 295 _cell_measurement_theta_max 60.538 _cell_measurement_theta_min 4.322 _cell_volume 1175.36(18) _computing_cell_refinement ; SAINT (2013) V8.40A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_collection ; APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_reduction ; SAINT (2013) V8.40A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 295 _diffrn_detector 'CMOS Area detector' _diffrn_detector_area_resol_mean 10.24 _diffrn_detector_type 'Bruker Photon 100 CMOS Detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker Venture Metaljet' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_collimation 'Focusing mirrors' _diffrn_radiation_monochromator 'Helios MX Mirror Optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_unetI/netI 0.0222 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 18788 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 60.597 _diffrn_reflns_theta_min 2.761 _diffrn_source 'Metal Jet' _diffrn_source_current 2.86 _diffrn_source_power 0.199914 _diffrn_source_target Ga _diffrn_source_type 'Gallium Liquid Metal Jet Source' _diffrn_source_voltage 69.9 _exptl_absorpt_coefficient_mu 9.887 _exptl_absorpt_correction_T_max 0.2850 _exptl_absorpt_correction_T_min 0.1630 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1386 before and 0.0521 after correction. The Ratio of minimum to maximum transmission is 0.5719. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light Colorless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.307 _exptl_crystal_description plate _exptl_crystal_F_000 816 _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Venture diffractometer equipped with a Photon 100 CMOS Detector, a Helios MX optics and a Kappa goniometer. The crystal-to-detector distance was 4.0 cm, and the data collection was carried out in 1024 x 1024 pixel mode. ; _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. ; _refine_diff_density_max 0.300 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.060 _refine_ls_extinction_coef 0.00054(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2019/2 (Sheldrick 2019)' _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 212 _refine_ls_number_reflns 2680 _refine_ls_number_restraints 11 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0207 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.3989P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.0555 _refine_special_details ; 1. Restrained distances O1-H1 0.82 with sigma of 0.002 O3-H3 0.82 with sigma of 0.002 O5-H5 0.82 with sigma of 0.002 O4-H4 0.82 with sigma of 0.002 O6-H6 0.82 with sigma of 0.002 O7-H7 0.82 with sigma of 0.002 O8-H8 0.82 with sigma of 0.002 O9-H9 0.82 with sigma of 0.002 O10-H10 0.82 with sigma of 0.002 O11-H11 0.82 with sigma of 0.002 O12-H12 0.82 with sigma of 0.002 2. Others Fixed Sof: H1(0.5) H2(0.5) H3(0.5) H4(0.5) H6(0.5) H5(0.5) H9(0.5) H7(0.5) H8(0.5) H10(0.5) H11(0.5) H12(0.5) _shelx_SHELXL_version_number '2019/3' ; _reflns_Friedel_coverage 0.000 _reflns_number_gt 2423 _reflns_number_total 2680 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file mix9.cif _cod_data_source_block mix9 _cod_database_code 3500142 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.83662(3) 0.58524(9) 0.43490(2) 0.02210(10) Uani 1 1 d . . . . . P2 P 0.82646(3) 0.48158(8) 0.68484(2) 0.02163(10) Uani 1 1 d . . . . . P3 P 0.48477(2) 0.37928(9) 0.61821(2) 0.02195(10) Uani 1 1 d . . . . . O1 O 0.93661(8) 0.4687(3) 0.43947(7) 0.0352(3) Uani 1 1 d D . . . . H1 H 0.971(3) 0.489(12) 0.4831(9) 0.052(14) Uiso 0.5 1 d D . P . . O2 O 0.81008(9) 0.8351(3) 0.37757(6) 0.0281(2) Uani 1 1 d . . . . . H2 H 0.795(4) 0.963(11) 0.388(3) 0.053(17) Uiso 0.5 1 d . . P A 2 O3 O 0.76266(8) 0.3340(3) 0.41024(7) 0.0305(2) Uani 1 1 d D . . . . H3 H 0.788(2) 0.179(4) 0.404(2) 0.024(9) Uiso 0.5 1 d D . P B 1 O4 O 0.83657(8) 0.7061(3) 0.51217(6) 0.0299(2) Uani 1 1 d D . . . . H4 H 0.846(3) 0.568(6) 0.5419(18) 0.043(12) Uiso 0.5 1 d D . P C 1 H6 H 0.846(4) 0.485(7) 0.587(2) 0.062(16) Uiso 0.5 1 d D . P D 2 O5 O 0.72424(8) 0.6123(3) 0.65970(7) 0.0340(3) Uani 1 1 d D . . . . H5 H 0.6809(18) 0.489(6) 0.647(2) 0.032(10) Uiso 0.5 1 d D . P E 1 H9 H 0.623(2) 0.401(6) 0.643(3) 0.050(13) Uiso 0.5 1 d D . P F 2 O6 O 0.84985(9) 0.3481(3) 0.61693(6) 0.0319(3) Uani 1 1 d D . . . . O7 O 0.89644(7) 0.7286(2) 0.72066(6) 0.0276(2) Uani 1 1 d D . . . . H7 H 0.870(3) 0.883(5) 0.727(3) 0.048(13) Uiso 0.5 1 d D . P G 2 O8 O 0.83303(9) 0.2297(2) 0.74185(6) 0.0301(2) Uani 1 1 d D . . . . H8 H 0.853(3) 0.068(4) 0.733(2) 0.032(11) Uiso 0.5 1 d D . P H 1 O9 O 0.58693(7) 0.2573(3) 0.63191(6) 0.0295(2) Uani 1 1 d D . . . . O10 O 0.48604(8) 0.6303(2) 0.67342(6) 0.0285(2) Uani 1 1 d D . . . . H10 H 0.457(3) 0.779(6) 0.654(2) 0.048(13) Uiso 0.5 1 d D . P I 2 O11 O 0.42029(8) 0.1282(2) 0.63025(7) 0.0287(2) Uani 1 1 d D . . . . H11 H 0.451(2) -0.023(5) 0.646(2) 0.032(10) Uiso 0.5 1 d D . P J 1 O12 O 0.44282(8) 0.4873(3) 0.53650(6) 0.0316(3) Uani 1 1 d D . . . . H12 H 0.485(2) 0.493(11) 0.516(2) 0.042(12) Uiso 0.5 1 d D . P K -1 K1 K 0.99203(2) 0.01912(8) 0.36394(2) 0.03040(10) Uani 1 1 d . . . . . K2 K 0.65791(2) 0.57770(9) 0.26483(2) 0.03192(10) Uani 1 1 d . . . . . K3 K 0.68098(3) 1.03817(9) 0.52260(2) 0.03434(10) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.02166(18) 0.0214(2) 0.02269(18) -0.00055(14) 0.00607(13) 0.00202(13) P2 0.02250(18) 0.01921(19) 0.02381(18) -0.00080(14) 0.00808(14) 0.00102(13) P3 0.02204(18) 0.0211(2) 0.02283(19) 0.00155(14) 0.00707(13) 0.00015(13) O1 0.0225(5) 0.0483(7) 0.0313(6) -0.0130(6) 0.0033(5) 0.0079(5) O2 0.0374(6) 0.0222(6) 0.0254(6) 0.0010(5) 0.0107(5) -0.0009(5) O3 0.0280(5) 0.0213(6) 0.0424(7) -0.0003(5) 0.0111(5) -0.0005(5) O4 0.0386(6) 0.0290(6) 0.0238(5) -0.0001(5) 0.0122(5) 0.0082(5) O5 0.0220(5) 0.0296(6) 0.0486(7) -0.0032(5) 0.0082(5) 0.0021(5) O6 0.0456(7) 0.0287(6) 0.0248(5) 0.0021(5) 0.0155(5) 0.0088(5) O7 0.0249(5) 0.0214(5) 0.0354(6) 0.0004(5) 0.0077(4) -0.0013(4) O8 0.0451(6) 0.0197(6) 0.0300(6) 0.0010(5) 0.0182(5) -0.0004(5) O9 0.0215(5) 0.0285(6) 0.0375(6) 0.0047(5) 0.0078(4) 0.0026(4) O10 0.0358(6) 0.0216(6) 0.0262(6) -0.0011(5) 0.0069(4) -0.0001(5) O11 0.0259(5) 0.0207(6) 0.0405(6) 0.0011(5) 0.0118(5) -0.0012(4) O12 0.0273(5) 0.0455(7) 0.0234(5) 0.0067(5) 0.0101(4) 0.0082(5) K1 0.02932(17) 0.03141(19) 0.03293(18) -0.00262(14) 0.01324(14) 0.00103(13) K2 0.03015(17) 0.0393(2) 0.02564(17) -0.00145(14) 0.00762(13) -0.00270(14) K3 0.02993(18) 0.0349(2) 0.03493(19) -0.00599(15) 0.00527(14) 0.00502(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3778 0.8310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2543 0.3332 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 P1 O3 109.67(7) . . O1 P1 O4 110.20(6) . . O2 P1 O1 108.93(7) . . O2 P1 O3 109.36(7) . . O2 P1 O4 108.98(7) . . O3 P1 O4 109.69(7) . . O5 P2 O8 109.88(7) . . O6 P2 O5 109.92(7) . . O6 P2 O8 107.58(6) . . O7 P2 O5 108.23(6) . . O7 P2 O6 111.05(7) . . O7 P2 O8 110.18(7) . . O9 P3 O12 110.30(6) . . O10 P3 O9 110.11(7) . . O10 P3 O11 109.03(6) . . O10 P3 O12 110.80(7) . . O11 P3 O9 108.80(6) . . O11 P3 O12 107.74(7) . . P1 O1 H1 107(4) . . P1 O2 H2 118(5) . . P1 O3 H3 111(2) . . P1 O4 H4 109(3) . . P2 O5 H5 115(3) . . P2 O6 H6 106(3) . . P2 O7 H7 114(3) . . P2 O8 H8 117(3) . . P3 O9 H9 106(3) . . P3 O10 H10 114(3) . . P3 O11 H11 111(3) . . P3 O12 H12 110(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 P1 O1 1.5328(11) . P1 O2 1.5214(12) . P1 O3 1.5361(12) . P1 O4 1.5460(11) . P2 O5 1.5406(11) . P2 O6 1.5380(11) . P2 O7 1.5216(11) . P2 O8 1.5409(12) . P3 O9 1.5389(11) . P3 O10 1.5288(12) . P3 O11 1.5348(11) . P3 O12 1.5406(11) . O1 H1 0.820(2) . O2 H2 0.67(5) . O3 H3 0.820(2) . O4 H4 0.820(2) . O5 H5 0.820(2) . O6 H6 0.820(2) . O7 H7 0.820(2) . O8 H8 0.820(2) . O9 H9 0.820(2) . O10 H10 0.820(2) . O11 H11 0.820(2) . O12 H12 0.820(2) . K2 H2 3.08(5) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1 H1 O1 0.820(2) 1.662(14) 2.462(2) 165(5) 3_766 yes O2 H2 O3 0.67(5) 1.82(5) 2.4856(17) 173(6) 1_565 yes O3 H3 O2 0.820(2) 1.685(10) 2.4856(17) 165(4) 1_545 yes O4 H4 O6 0.820(2) 1.703(12) 2.5009(16) 164(4) . yes O6 H6 O4 0.820(2) 1.695(11) 2.5009(16) 167(5) . yes O5 H5 O9 0.820(2) 1.682(7) 2.4954(16) 171(4) . yes O9 H9 O5 0.820(2) 1.708(15) 2.4954(16) 161(4) . yes O7 H7 O8 0.820(2) 1.707(7) 2.5202(16) 171(5) 1_565 yes O8 H8 O7 0.820(2) 1.702(4) 2.5202(16) 176(4) 1_545 yes O10 H10 O11 0.820(2) 1.677(12) 2.4775(16) 165(4) 1_565 yes O11 H11 O10 0.820(2) 1.676(10) 2.4775(16) 165(4) 1_545 yes O12 H12 O12 0.820(2) 1.657(7) 2.470(2) 171(5) 3_666 yes _cod_database_fobs_code 3500142