Invitation to Submit: The Cambridge Structural Database " A peculiar dehydration and solid-solid phase transition of the active pharmaceutical ingredient AZD9898 based on in situ single crystal-to-single crystal transformations "
Pettersen, Anna; Putra, Okky Dwichandra; Light, Mark E.; Namatame, Yukiko; CrystEngComm  (2020) –; doi:10.1039/D0CE00276C

data_7240200
_publ_section_title
;
 Invitation to Submit: The Cambridge Structural Database " A peculiar
 dehydration and solid-solid phase transition of the active pharmaceutical
 ingredient AZD9898 based on in situ single crystal-to-single crystal
 transformations "
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00276C
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C20 H19 Cl F3 N3 O4), 0.5(H2 O)'
_chemical_formula_sum            'C40 H39 Cl2 F6 N6 O8.5'
_chemical_formula_weight         924.66
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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
_audit_update_record
;
2020-02-07 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                103.378(3)
_cell_angle_beta                 105.493(3)
_cell_angle_gamma                104.407(3)
_cell_formula_units_Z            1
_cell_length_a                   9.0757(3)
_cell_length_b                   11.0502(4)
_cell_length_c                   11.7199(5)
_cell_measurement_reflns_used    10496
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.698
_cell_measurement_theta_min      3.109
_cell_volume                     1039.69(8)
_computing_cell_refinement
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 (Rigaku, 2013)'
_computing_data_reduction
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_pressure         101.3
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC12 FRE-VHF'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25300
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.698
_diffrn_reflns_theta_min         3.109
_diffrn_source                   'Rotating anode'
_diffrn_source_type              'Rotating anode'
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       plate
_exptl_crystal_F_000             477
_exptl_crystal_recrystallization_method
'the material was recrystallized from --- by slow evaporation'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 3447 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         10496
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0596P)^2^+0.0049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                8772
_reflns_number_total             10496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00276c2.cif
_cod_data_source_block           2016scas0001_R_100K
_cod_original_cell_volume        1039.68(7)
_cod_original_formula_sum        'C40 H39 Cl2 F6 N6 O8.50'
_cod_database_code               7240200
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              1527