Exploring the polymorphism of sofosbuvir via mechanochemistry: effect of milling jar geometry and material
Chatziadi, Argyro; Skořepová, Eliška; Kohout, Martin; Ridvan, Luděk; Šoóš, Miroslav; CrystEngComm  (2022) –; doi:10.1039/D1CE01561C

data_7244520
_publ_section_title
;
 Exploring the polymorphism of sofosbuvir via mechanochemistry: effect of
 milling jar geometry and material
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01561C
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H29 F N3 O9 P, H2 O'
_chemical_formula_sum            'C22 H31 F N3 O10 P'
_chemical_formula_weight         547.48
_chemical_name_systematic        'sofosbuvir hydrate'
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2021-09-17 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.187550(8)
_cell_length_b                   13.996380(9)
_cell_length_c                   20.528931(11)
_cell_measurement_reflns_used    41742
_cell_measurement_temperature    120
_cell_measurement_theta_max      68
_cell_measurement_theta_min      4
_cell_volume                     2639.865(3)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_pressure         100
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.067
_diffrn_reflns_av_unetI/netI     0.061
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57181
_diffrn_reflns_theta_full        67.595
_diffrn_reflns_theta_max         67.595
_diffrn_reflns_theta_min         3.822
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.505
_exptl_absorpt_correction_T_max  0.58
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
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_exptl_crystal_size_mid          0.466
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_refine_diff_density_min         -0.27
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 2030 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.027(6)
_refine_ls_extinction_coef       90(6)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0189
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4741
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.0006886
_refine_ls_shift/su_mean         0.0000419
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.85P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0747
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0747
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                4694
_reflns_number_total             4741
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.94
_oxford_diffrn_Wilson_scale      0.06
_oxford_refine_ls_r_factor_ref   0.0290
_oxford_refine_ls_scale          3.96(4)
_oxford_reflns_number_all        4741
_cod_data_source_file            d1ce01561c2.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

2025-03-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         273.74
_cod_original_formula_moiety         'C11 H15.50 F0.50 N1.50 O5 P0.50'
_cod_original_formula_units_Z            8
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C11 H15.50 F0.50 N1.50 O5 P0.50'
_cod_database_code               7244520
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_hooft_y                  0.023(6)
_oxford_bijvoet_difference       0.027(6)
_oxford_refined_flack_x          0.034(17)