Structural Analysis of Metastable Pharmaceutical Loratadine Form II, by 3D Electron Diffraction and DFT+D Energy Minimisation
Woollam, Grahame R.; Das, Partha P.; Mugnaioli, Enrico; Andrusenko, Iryna; Galanis, Athanassios S.; van de Streek, Jacco; Nicolopoulos, Stavros; Gemmi, Mauro; Wagner, Trixie; CrystEngComm  (2020) –; doi:10.1039/D0CE01216E

data_7241344
_publ_section_title
;
 Structural Analysis of Metastable Pharmaceutical Loratadine Form II, by
 3D Electron Diffraction and DFT+D Energy Minimisation
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01216E
_journal_year                    2020
_chemical_formula_sum            'C22 H23 Cl N2 O2'
_chemical_formula_weight         382.89
_chemical_name_common            Claritin
_chemical_name_systematic        Loratadine
_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_type_scat_source           'Doyle & Turner (1968)'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-09-28 deposited with the CCDC.	2020-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.2(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.4(7)
_cell_length_b                   5.28(11)
_cell_length_c                   22.6(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3723(14)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR2014 (Burla et al. 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'single-electron detector MEDIPIX'
_diffrn_detector_type            'ASI Timepix'
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device       'transmission electron microscope'
_diffrn_measurement_device_type  'Zeiss Libra 120'
_diffrn_measurement_method
'stepwise energy-filtered and precession-assisted 3D electron diffraction'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0335
_diffrn_reflns_av_R_equivalents  0.2497
_diffrn_reflns_av_unetI/netI     0.1862
_diffrn_reflns_Laue_measured_fraction_full 0.862
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3350
_diffrn_reflns_point_group_measured_fraction_full 0.862
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        0.887
_diffrn_reflns_theta_max         0.887
_diffrn_reflns_theta_min         0.062
_diffrn_source                   '120 kV electron microscope'
_diffrn_source_type              'LaB6 gun'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       nanocrystal
_exptl_crystal_F_000             627
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene/TBME'
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.488
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1320
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      3.424
_refine_ls_R_factor_all          0.5758
_refine_ls_R_factor_gt           0.5807
_refine_ls_shift/su_max          2.158
_refine_ls_shift/su_mean         0.118
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.8072
_refine_ls_wR_factor_ref         0.8195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1112
_reflns_number_total             1320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01216e2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        3717(131)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7241344
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              60000