Modulating the solubility and pharmacokinetic property of 5-fluorouracil via cocrystals
Dai, Xia-Lin; Wu, Chao; Li, Jin-Hui; Liu, Lian-Chao; He, Xin; Lu, Tong-Bu; Chen, Jia-Mei; CrystEngComm  (2020) –; doi:10.1039/D0CE00409J

data_7240383
_publ_section_title
;
 Modulating the solubility and pharmacokinetic property of 5-fluorouracil
 via cocrystals
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00409J
_journal_year                    2020
_chemical_formula_moiety         'C4 H3 F N2 O2, C7 H6 O4'
_chemical_formula_sum            'C11 H9 F N2 O6'
_chemical_formula_weight         284.20
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-09 deposited with the CCDC.	2020-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                111.550(7)
_cell_angle_beta                 107.076(7)
_cell_angle_gamma                100.662(6)
_cell_formula_units_Z            2
_cell_length_a                   7.8352(6)
_cell_length_b                   8.9191(7)
_cell_length_c                   9.4663(7)
_cell_measurement_reflns_used    3598
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      78.5570
_cell_measurement_theta_min      5.4680
_cell_volume                     555.34(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -28.00  68.00   0.50    0.50    --    0.00  57.00-150.00  192
  2  \w    -29.00  41.00   0.50    0.50    --    0.00  37.00   0.00  140
  3  \w     51.00  85.00   0.50    0.50    --    0.00  37.00   0.00   68
  4  \w    -27.00  10.00   0.50    0.50    --    0.00  57.00 120.00   74
  5  \w     75.00 113.00   0.50    0.50    --  106.20 -82.00 150.00   76
  6  \w     95.00 124.00   0.50    0.50    --  106.20  61.00-150.00   58
  7  \w     96.00 141.00   0.50    0.50    --  106.20  45.00-180.00   90
  8  \w     20.00  68.00   0.50    0.50    --  106.20 -45.00-120.00   96
  9  \w    106.00 132.00   0.50    0.50    --  106.20 -77.00 -90.00   52
 10  \w     33.00  73.00   0.50    0.50    --  106.20 -82.00 -30.00   80
 11  \w     82.00 148.00   0.50    0.50    --  106.20  45.00-150.00  132
 12  \w     80.00 179.00   0.50    0.50    --  106.20  45.00 150.00  198
 13  \w     38.00 137.00   0.50    0.50    --  106.20 -82.00  60.00  198
 14  \w    122.00 196.00   0.50    0.50    --  106.20  45.00  60.00  148
 15  \w     37.00  70.00   0.50    0.50    --  106.20 -82.00-120.00   66
 16  \w     17.00  91.00   0.50    0.50    --  106.20 -77.00 -90.00  148
 17  \w     86.00 162.00   0.50    0.50    --  106.20  45.00 120.00  152
 18  \w     78.00 132.00   0.50    0.50    --  106.20 -82.00-120.00  108
 19  \w    171.00 196.00   0.50    0.50    --  106.20  61.00-150.00   50
 20  \w     78.00 134.00   0.50    0.50    --  106.20 -45.00-120.00  112
 21  \w    150.00 192.00   0.50    0.50    --  106.20  45.00-180.00   84
 22  \w     90.00 130.00   0.50    0.50    --  106.20 -82.00 -30.00   80
 23  \w     96.00 141.00   0.50    0.50    --  106.20 -77.00  30.00   90
 24  \w    153.00 191.00   0.50    0.50    --  106.20  45.00-150.00   76
 25  \w     28.00  54.00   0.50    0.50    --  106.20 -77.00  30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0968933000
_diffrn_orient_matrix_UB_12      0.0298948000
_diffrn_orient_matrix_UB_13      0.1231715000
_diffrn_orient_matrix_UB_21      0.1941652000
_diffrn_orient_matrix_UB_22      0.0696631000
_diffrn_orient_matrix_UB_23      0.1443483000
_diffrn_orient_matrix_UB_31      0.0192005000
_diffrn_orient_matrix_UB_32      0.1814906000
_diffrn_orient_matrix_UB_33      0.0169744000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5446
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.650
_diffrn_reflns_theta_min         5.471
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       block
_exptl_crystal_F_000             292
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0900
_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^)+(0.1971P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2227
_refine_ls_wR_factor_ref         0.2295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2062
_reflns_number_total             2323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00409j2.cif
_cod_data_source_block           5FU-35DHBA
_cod_original_cell_volume        555.34(8)
_cod_database_code               7240383
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C6(H6A), C8(H8), C10(H10), C4(H4A)
2.b Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O6(H6)
;
_shelx_res_checksum              67071
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.602
_oxdiff_exptl_absorpt_empirical_full_min 0.485