Potassium Dihydrogen Phosphate - Monoclinic Form at 150 K / Ambient Pressure
Thierry Maris; Personal communication to COD  (2025) –; doi:

data_3500142
_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
_cod_database_fobs_code 3500142