Crystal structure of a new hydrate form of the NSAID sodium diclofenac
Angel Nieto, Ismael; Bernès, Sylvain; Pérez-Benítez, Aarón; Acta Crystallographica Section E 76 (2020) 1846–1850; doi:10.1107/S2056989020015108

data_2243680
_publ_section_title
;
 Crystal structure of a new hydrate form of the NSAID sodium diclofenac
;
_journal_coeditor_code           JY2003
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1846
_journal_page_last               1850
_journal_paper_doi               10.1107/S2056989020015108
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac
'[Na2 (C14 H10 Cl2 N O2) (H2 O)7] (C14 H10 Cl2 N O2)'
_chemical_formula_moiety
'C14 H24 Cl2 N Na2 O9 +, C14 H10 Cl2 N O2 -'
_chemical_formula_sum            'C28 H34 Cl4 N2 Na2 O11'
_chemical_formula_weight         762.35
_chemical_name_common            'Sodium diclofenac 3.5-hydrate'
_chemical_name_systematic
;Tetra-\m-aqua-\k^8^<i>O</i>:<i>O</i>-decaaquabis{\m~3~-2-[2-(2,6-dichloroanilino)phenyl]acetato-\k^3^<i>O</i>:<i>O</i>:<i>O</i>}tetrasodium(I)
bis{2-[2-(2,6-dichloroanilino)phenyl]acetate}
;
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90.331(4)
_cell_angle_beta                 99.828(4)
_cell_angle_gamma                90.436(4)
_cell_formula_units_Z            2
_cell_length_a                   9.4370(4)
_cell_length_b                   9.5675(5)
_cell_length_c                   19.1526(10)
_cell_measurement_reflns_used    29092
_cell_measurement_temperature    295.0(10)
_cell_measurement_theta_max      22.58
_cell_measurement_theta_min      2.38
_cell_volume                     1703.79(15)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2019)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2019)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2019)
;
_computing_molecular_graphics
;
XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2020)
;
_computing_publication_material
;
publCif (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      295.0(10)
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.1009
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51408
_diffrn_reflns_theta_full        19.664
_diffrn_reflns_theta_max         20.503
_diffrn_reflns_theta_min         2.421
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_current           0.55
_diffrn_source_power             0.039
_diffrn_source_voltage           65
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-AREA; Stoe & Cie, 2019)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       prism
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.844
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         6930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.844
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                3920
_reflns_number_total             6930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jy2003sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2023-01-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C56 H68 Cl8 N4 Na4 O22'
_cod_original_formula_weight         1524.70
_cod_original_formula_moiety
'C28 H48 Cl4 N2 Na4 O18 2+, 2(C14 H10 Cl2 N O2 -)'
_cod_original_formula_iupac
'[Na4 (C14 H10 Cl2 N O2)2 (H2 O)14] (C14 H10 Cl2 N O2)2'
_cod_original_formula_units_Z            1
_cod_database_code               2243680
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.987
_shelx_hkl_checksum              30201
_shelx_res_checksum              91471
_cod_database_fobs_code 2243680