Diclofenac solubility: independent determination of the intrinsic solubility of three crystal forms.
Llinàs, Antonio; Burley, Jonathan C.; Box, Karl J.; Glen, Robert C.; Goodman, Jonathan M.; Journal of medicinal chemistry 50 (2007) 979–983; doi:10.1021/jm0612970

data_1505019
_publ_section_title
;
 Diclofenac solubility: independent determination of the intrinsic
 solubility of three crystal forms.
;
_journal_issue                   5
_journal_name_full               'Journal of medicinal chemistry'
_journal_page_first              979
_journal_page_last               983
_journal_paper_doi               10.1021/jm0612970
_journal_volume                  50
_journal_year                    2007
_chemical_formula_moiety         '4(C14 H10 Cl2 N O2 1-),4(Na 1+),19(H2 O)'
_chemical_formula_sum            'C14 H19.5 Cl2 N Na O6.75'
_chemical_formula_weight         403.69
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.7290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.55400(10)
_cell_length_b                   39.4910(4)
_cell_length_c                   9.84120(10)
_cell_measurement_reflns_used    40474
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     3712.75(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;

 HKL Denzo and Scalepack (Otwinowski & Minor 1997)

;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.865
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20123
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

multi-scan from symmetry-related measurements 

 Sortav (Blessing 1995)

;
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1008
_refine_ls_number_reflns         11098
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.274
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+1.3068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                10739
_reflns_number_total             11098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jm0612970si20061219_020352.cif
_cod_data_source_block           jg0501
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               1505019