Crystal structure of the non-steroidal anti-inflammatory drug (NSAID) tolmetin sodium
Konovalova, Irina S.; Kovalenko, Sergiy M.; Kravchenko, Dmitry V.; Chuev, Vladimir P.; Acta Crystallographica Section E 77 (2021) 134–137; doi:10.1107/S2056989021000414

data_2243729
_publ_section_title
;
 Crystal structure of the non-steroidal anti-inflammatory drug (NSAID)
 tolmetin sodium
;
_journal_coeditor_code           ZQ2259
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              134
_journal_page_last               137
_journal_paper_doi               10.1107/S2056989021000414
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '2Na +, 2C15 H14 N1 O3 -, 4H2 O1'
_chemical_formula_moiety         '2(Na +), 2(C15 H14 N1 O3 -), 4(H2 O1)'
_chemical_formula_sum            'C30 H36 N2 Na2 O10'
_chemical_formula_weight         630.59
_chemical_name_systematic
;
Sodium
2-[1-methyl-5-(4-methylbenzoyl)-1<i>H</i>-pyrrol-2-yl]acetate dihydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     geom
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                92.922(8)
_cell_angle_beta                 98.873(7)
_cell_angle_gamma                113.038(9)
_cell_formula_units_Z            2
_cell_length_a                   8.5404(8)
_cell_length_b                   9.0144(9)
_cell_length_c                   21.6217(19)
_cell_measurement_reflns_used    1420
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      3.1
_cell_volume                     1502.1(3)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
ShelXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction Xcalibur, Sapphire3'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11985
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.882
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2018)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0844P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1910
_reflns_number_gt                3288
_reflns_number_total             5283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zq2259sup1.cif
_cod_data_source_block           I
_cod_database_code               2243729
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.987
_cod_database_fobs_code 2243729