Potassium salts of hypodiphosphoric acid
Szafranowska, Barbara; Ślepokura, Katarzyna; Lis, Tadeusz; Acta Crystallographica Section C 68 (2012) i71–i82; doi:10.1107/S010827011204317X

data_2018713
_publ_section_title
;
 Potassium salts of hypodiphosphoric acid
;
_journal_coeditor_code           FN3115
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i71
_journal_page_last               i82
_journal_paper_doi               10.1107/S010827011204317X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '3K + , H O6 P2 3- , 4H2 O'
_chemical_formula_moiety         '3(K +), H O6 P2 3-, 4(H2 O)'
_chemical_formula_sum            'H9 K3 O10 P2'
_chemical_formula_weight         348.31
_chemical_name_systematic
;
Tripotassium hydrogen hypodiphosphate tetrahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.82(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.743(3)
_cell_length_b                   15.725(6)
_cell_length_c                   14.418(6)
_cell_measurement_reflns_used    15980
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      38.63
_cell_measurement_theta_min      4.31
_cell_volume                     2206.3(14)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_device_type
'Oxford Xcalibur PX \k-geometry diffractometer with an Onyx CCD camera'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35056
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         38.63
_diffrn_reflns_theta_min         4.31
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.576
_refine_ls_extinction_coef       0.00172(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         10230
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0080P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0458
_reflns_number_gt                5268
_reflns_number_total             10230
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3115.cif
_cod_data_source_block           V
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018713
_cod_database_fobs_code          2018713