A new olanzapine cocrystal obtained from volatile deep eutectic solvents and determined by 3D electron diffraction
Andrusenko, Iryna; Potticary, Jason; Hall, Simon R.; Gemmi, Mauro; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620012779

data_2108733
_publ_section_title
;
 A new olanzapine cocrystal obtained from volatile deep eutectic solvents
 and determined by 3D electron diffraction
;
_journal_coeditor_code           JE5035SUP1
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620012779
_journal_volume                  76
_journal_year                    2020
_chemical_formula_sum            'C23 H26 N4 O S'
_chemical_formula_weight         406.55
_chemical_name_systematic        'C17 H20 N4 S, C6 H6 O'
_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   geom
_atom_type_scat_source           'Doyle & Turner (1968)'
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                96.683(4)
_cell_angle_beta                 95.288(3)
_cell_angle_gamma                104.474(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4054(8)
_cell_length_b                   10.4228(11)
_cell_length_c                   11.9607(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1118.59(17)
_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 0.542
_diffrn_measured_fraction_theta_max 0.542
_diffrn_measurement_device       'transmission electron microscope'
_diffrn_measurement_device_type  'Zeiss Libra 120'
_diffrn_measurement_method
'stepwise precession-assisted 3D electron diffration'
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0335
_diffrn_reflns_av_R_equivalents  0.1511
_diffrn_reflns_av_unetI/netI     0.1608
_diffrn_reflns_Laue_measured_fraction_full 0.542
_diffrn_reflns_Laue_measured_fraction_max 0.542
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2485
_diffrn_reflns_point_group_measured_fraction_full 0.542
_diffrn_reflns_point_group_measured_fraction_max 0.542
_diffrn_reflns_theta_full        0.960
_diffrn_reflns_theta_max         0.960
_diffrn_reflns_theta_min         0.081
_diffrn_source                   '120 kV electron microscope'
_diffrn_source_type              'LaB6 gun'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       nanocrystal
_exptl_crystal_F_000             170
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1269
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      2.984
_refine_ls_R_factor_all          0.3896
_refine_ls_R_factor_gt           0.3140
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5996
_refine_ls_wR_factor_ref         0.6255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                720
_reflns_number_total             1269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            je5035sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1118.58(17)
_cod_database_code               2108733
_cod_database_fobs_code          2108733
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              21492
_shelx_hkl_checksum              51371