A threefold superstructure of the anti-epileptic drug phenytoin sodium as a mixed methanol solvate hydrate
Shah, Harsh S.; Chaturvedi, Kaushalendra; Zeller, Matthias; Bates, Simon; Morris, Kenneth; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619010696

data_2021740
_publ_section_title
;
 A threefold superstructure of the anti-epileptic drug phenytoin sodium as
 a mixed methanol solvate hydrate
;
_journal_coeditor_code           SK3736
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619010696
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Na (C15 H11 N2 O2) (C H4 O) (H2 O)0.36]'
_chemical_formula_moiety         'C16 H15.72 N2 Na O3.36'
_chemical_formula_sum            'C16 H15.72 N2 Na O3.36'
_chemical_formula_weight         312.78
_chemical_name_systematic
Poly[aquatris(\m~3~-4,4-diphenyl-2,5-dioxoimidazolidin-1-ido)trimethanoltrisodium(I)]
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 106.0770(12)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   15.9687(3)
_cell_length_b                   18.7065(4)
_cell_length_c                   15.8249(4)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      80.0535
_cell_measurement_theta_min      2.8792
_cell_volume                     4542.31(18)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015, 2018) and
SHELXLE (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30401
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.353
_diffrn_reflns_theta_min         2.880
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       rod
_exptl_crystal_F_000             1963
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.426
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         9389
_refine_ls_number_restraints     856
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+1.3413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1577
_reflns_number_gt                7343
_reflns_number_total             9389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3736sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2023-05-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C48 H47.16 N6 Na3 O10.08'
_cod_original_formula_weight         938.33
_cod_original_formula_moiety         'C48 H47.16 N6 Na3 O10.08'
_cod_original_formula_iupac       '[Na3 (C15 H11 N2 O2)3 (C H4 O)3 (H2 O)1.08]'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        4542.31(17)
_cod_database_code               2021740
_shelx_estimated_absorpt_t_min   0.810
_shelx_estimated_absorpt_t_max   0.876
_shelx_hkl_checksum              57162
_shelx_res_checksum              29543
_cod_database_fobs_code 2021740