Solid-State Properties and Dehydration Behavior of the Active Pharmaceutical Ingredient Potassium Guaiacol-4-sulfonate
Mahé, Nathalie; Nicolaï, Béatrice; Barrio, Maria; Perrin, Marc-Antoine; Do, Bernard; Tamarit, Josep-Lluis; Céolin, René; Rietveld, Ivo B.; Crystal Growth & Design 13 (2013) 3028–; doi:10.1021/cg400427v

data_4510719
_publ_section_title
;
 Solid-State Properties and Dehydration Behavior of the Active
 Pharmaceutical Ingredient Potassium Guaiacol-4-sulfonate
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3028
_journal_paper_doi               10.1021/cg400427v
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         C7O5H7S1K1,0.5H2O
_chemical_formula_sum            'C7 H8 K O5.5 S'
_chemical_formula_weight         251.30
_chemical_name_common
;
 potassium guaiacolsulfonate hemihydrate
;
_chemical_name_systematic
;
 potassium 4-hydroxy-3-methoxybenzenesulfonate hemihydrate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.1560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.4360(16)
_cell_length_b                   6.3452(5)
_cell_length_c                   16.2640(14)
_cell_measurement_temperature    298(2)
_cell_volume                     1990.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Smart-Apex CCD Bruker AXS'
_diffrn_measurement_method       '\f and \w'
_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  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5862
_diffrn_reflns_theta_full        23.24
_diffrn_reflns_theta_max         23.24
_diffrn_reflns_theta_min         2.11
_diffrn_standards_interval_time  30
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  0.9295
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1427
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0263P)^2^+1.7677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                1370
_reflns_number_total             1427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400427v_si_003.cif
_cod_data_source_block           guaiacolsulfonatepotassium
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

2022-02-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C14 H16 K2 O11 S2'
_cod_original_formula_weight         502.61
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4510719