Structure Elucidation of Olanzapine Molecular Salts by Combining Mechanochemistry and Micro-Electron Diffraction
Gogoi, Diptajyoti; Sasaki, Toshiyuki; Nakane, Takanori; Kawamoto, Akihiro; Hojo, Hironobu; Kurisu, Genji; Thakuria, Ranjit; Crystal Growth & Design 23 (2023) 5821–5826; doi:10.1021/acs.cgd.3c00432

data_3000439
_publ_section_title
;
 Structure Elucidation of Olanzapine Molecular Salts by Combining
 Mechanochemistry and Micro-Electron Diffraction
;
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5821
_journal_page_last               5826
_journal_paper_doi               10.1021/acs.cgd.3c00432
_journal_volume                  23
_journal_year                    2023
_chemical_formula_moiety         'C22 H30 N4 O5 S'
_chemical_formula_sum            'C22 H30 N4 O5 S'
_chemical_formula_weight         462.56
_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
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                78.613(2)
_cell_angle_beta                 80.880(3)
_cell_angle_gamma                87.127(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3239(4)
_cell_length_b                   9.8354(5)
_cell_length_c                   14.1883(7)
_cell_measurement_reflns_used    7280
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.55
_cell_measurement_theta_min      2.34
_cell_volume                     1124.11(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17353
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.601
_diffrn_reflns_theta_min         2.113
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS SADABS program'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0709P)^2^+0.2333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3836
_reflns_number_total             4661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            OLN-GA.cif
_cod_data_source_block           OLN_Glutarate_monohydrate
_cod_depositor_comments
'Releasing structure 3000439 into public domain as published material.'
_cod_database_code               3000439
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.974
_exptl_absorpt_special_details   'Sheldrick,G.M.,2015,University of gottingen'
_shelx_res_checksum              99202
_shelx_hkl_checksum              17927