Potassium hydrogen diphthalate dihydrate: a new structure and correction to the literature
Jason B. Benedict; Theresa Bullard; Werner Kaminsky; Bart Kahr; Acta Crystallographica Section C 60 (2004) m551–m553; doi:10.1107/S0108270104019043

data_2014551
_publ_section_title
;
 Potassium hydrogen diphthalate dihydrate: a new structure and
 correction to the literature
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m551
_journal_page_last               m553
_journal_paper_doi               10.1107/S0108270104019043
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'K +, C16 H11 O8 -, 2H2 O1'
_chemical_formula_moiety         'K +, C16 H11 O8 -, 2H2 O1'
_chemical_formula_sum            'C16 H15 K O10'
_chemical_formula_weight         406.38
_chemical_name_common            KAPdimerneedle
_chemical_name_systematic
;
Potassium hydrogen diphthalate dihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 116.5521(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5830(3)
_cell_length_b                   21.1270(5)
_cell_length_c                   6.8170(2)
_cell_measurement_reflns_used    239
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.4
_cell_measurement_theta_min      2.35
_cell_volume                     1749.93(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'KappaCCD Software (Nonius, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus (MacKat et al. 1998)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1994)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.806
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3680
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.89
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.9032
_exptl_absorpt_correction_T_min  0.8467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL2000 (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0522P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                1682
_reflns_number_total             2041
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq1160.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C16 H15 K1 O10'
_cod_database_code               2014551
_cod_database_fobs_code          2014551