Combined crystallographic and computational investigation of the solvent disorder present in a new tipiracil hydrochloride methanol solvate–hydrate
Barbas, Rafael; Font-Bardia, Mercè; de Sande, Dafne; Frontera, Antonio; Prohens, Rafel; CrystEngComm  (2022) –; doi:10.1039/D2CE00161F

data_7244748
_publ_section_title
;
 Combined crystallographic and computational investigation of the solvent
 disorder present in a new tipiracil hydrochloride methanol
 solvate--hydrate
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00161F
_journal_year                    2022
_chemical_absolute_configuration rm
_chemical_formula_moiety         '4(C9 H12 Cl N4 O2), C H4 O, 4(Cl), 3(H2 O)'
_chemical_formula_sum            'C37 H58 Cl8 N16 O12'
_chemical_formula_weight         1202.59
_chemical_name_systematic
'Tipiracil hydrochloride methanol solvate - hydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-30 deposited with the CCDC.	2022-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.1291(2)
_cell_length_b                   13.5358(5)
_cell_length_c                   27.2056(11)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.78
_cell_measurement_theta_min      2.70
_cell_volume                     2625.29(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            29776
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.782
_diffrn_reflns_theta_min         2.704
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.507
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 3473 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         10351
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+2.0267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.781
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                9186
_reflns_number_total             10351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00161f2.cif
_cod_data_source_block           023XB102A_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'direct methods' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7244748
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              38828