From formulation to structure: 3D electron diffraction for the structure solution of a new indomethacin polymorph from an amorphous solid dispersion.
Leung, Helen W.; Copley, Royston C. B.; Lampronti, Giulio I.; Day, Sarah J.; Saunders, Lucy K.; Johnstone, Duncan N.; Midgley, Paul A.; IUCrJ 11 (2024) –; doi:10.1107/S2052252524008121

data_1572415
_publ_section_title
;
 From formulation to structure: 3D electron diffraction for the structure
 solution of a new indomethacin polymorph from an amorphous solid
 dispersion.
;
_journal_coeditor_code           OF5005
_journal_issue                   5
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524008121
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         'C19 H16 Cl N O4'
_chemical_formula_sum            'C19 H16 Cl N O4'
_chemical_formula_weight         357.79
_chemical_name_common            indomethacin
_chemical_name_systematic
'[1-(4-chlorobenzoyl)-5-methoxy-2-methyl-1H-indol-3-yl]acetic acid'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 100.73(9)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   43.70(12)
_cell_length_b                   5.19(7)
_cell_length_c                   33.43(7)
_cell_measurement_reflns_used    6711
_cell_measurement_temperature    87(2)
_cell_measurement_theta_max      0.7060
_cell_measurement_theta_min      0.0790
_cell_volume                     7449(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'EPU-D 1.14.0.5171 (ThermoFisher)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Mercury 2021.3.0 (Build 333817)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution
'SHELXD, G.M.Sheldrick - Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.'
_diffrn_ambient_temperature      87(2)
_diffrn_measured_fraction_theta_full 0.780
_diffrn_measured_fraction_theta_max 0.770
_diffrn_measurement_device_type  'Thermo Scientific Krios G3i'
_diffrn_measurement_method       3D-ED
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0197
_diffrn_reflns_av_R_equivalents  0.1371
_diffrn_reflns_av_unetI/netI     0.1380
_diffrn_reflns_Laue_measured_fraction_full 0.780
_diffrn_reflns_Laue_measured_fraction_max 0.770
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            15410
_diffrn_reflns_point_group_measured_fraction_full 0.780
_diffrn_reflns_point_group_measured_fraction_max 0.770
_diffrn_reflns_theta_full        0.677
_diffrn_reflns_theta_max         0.705
_diffrn_reflns_theta_min         0.057
_diffrn_source                   'transmission electron microscope'
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            off-white
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       lath
_exptl_crystal_F_000             1114
_exptl_crystal_size_max          0.0070
_exptl_crystal_size_mid          0.0010
_exptl_crystal_size_min          0.0001
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       534(71)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         5885
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.3254
_refine_ls_R_factor_gt           0.2822
_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^)+(0.2913P)^2^+28.1400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.6107
_refine_ls_wR_factor_ref         0.6347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4062
_reflns_number_total             5885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            of5005.cif
_cod_data_source_block           I
_cod_original_cell_volume        7448(104)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1572415
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              81396
_shelx_hkl_checksum              2241