Exploring the solid form landscape of the antifungal drug isavuconazole: crystal structure analysis, phase transformation behavior and dissolution performance
Voronin, Alexander P.; Vasilev, Nikita A.; Surov, Artem O.; Churakov, Andrei V.; Perlovich, German L.; CrystEngComm 23 (2021) 8513–8526; doi:10.1039/D1CE01353J

data_7243935
_publ_section_title
;
 Exploring the solid form landscape of the antifungal drug isavuconazole:
 crystal structure analysis, phase transformation behavior and dissolution
 performance
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              8513
_journal_page_last               8526
_journal_paper_doi               10.1039/D1CE01353J
_journal_volume                  23
_journal_year                    2021
_chemical_absolute_configuration rmad
_chemical_formula_moiety
;
C22 H18 F2 N5 O S, C7 H7 O3 S, 0.212(C2 H3 N)
;
_chemical_formula_sum            'C29.42 H25.64 F2 N5.21 O4 S2'
_chemical_formula_weight         618.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-10-01 deposited with the CCDC.	2021-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.915(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.078(4)
_cell_length_b                   8.7230(12)
_cell_length_c                   12.0174(16)
_cell_measurement_reflns_used    3424
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.249
_cell_measurement_theta_min      2.438
_cell_volume                     3041.1(7)
_computing_cell_refinement       'SAINT (Bruker, 2018)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2016)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8833
_diffrn_reflns_point_group_measured_fraction_full 0.838
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.277
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       plate
_exptl_crystal_F_000             1283
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_exptl_transmission_factor_max   0.9281
_exptl_transmission_factor_min   0.5291
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 1213 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.08(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5000
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0789P)^2^+0.7051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.579
_reflns_Friedel_fraction_full    0.660
_reflns_Friedel_fraction_max     0.660
_reflns_number_gt                4268
_reflns_number_total             5000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01353j2.cif
_cod_data_source_block           z
_cod_depositor_comments
'Adding full bibliography for 7243935--7243938.cif.'
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7243935
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              89817
_shelx_hkl_checksum              84593