A 5-fluorouracil-kaempferol drug-drug cocrystal: ternary phase diagram, characterization and property evaluation
Lv, Wen-Ting; Liu, Xiao-Xu; Dai, Xia-Lin; Long, Xiangtian; Chen, Jia-Mei; CrystEngComm  (2020) –; doi:10.1039/D0CE01289K

data_7241408
_publ_section_title
;
 A 5-fluorouracil-kaempferol drug-drug cocrystal: ternary phase diagram,
 characterization and property evaluation
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01289K
_journal_year                    2020
_chemical_formula_moiety         'C4 H3 F N2 O2, C15 H10 O6'
_chemical_formula_sum            'C19 H13 F N2 O8'
_chemical_formula_weight         416.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-08 deposited with the CCDC.	2020-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.212(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.16340(10)
_cell_length_b                   17.9692(3)
_cell_length_c                   13.1115(2)
_cell_measurement_reflns_used    7103
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      79.0650
_cell_measurement_theta_min      4.1960
_cell_volume                     1655.51(5)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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      2.00  28.00   0.50    0.50    --    0.00  57.00-120.00   52
  2  \w    -14.00  88.00   0.50    0.50    --    0.00  57.00  30.00  204
  3  \w      3.00  79.00   0.50    0.50    --    0.00  57.00-150.00  152
  4  \w     78.00 140.00   0.50    0.50    --  106.20 -82.00 120.00  124
  5  \w     74.00 194.00   0.50    0.50    --  106.20  30.00  30.00  240
  6  \w     19.00  45.00   0.50    0.50    --  106.20 -77.00 -60.00   52
  7  \w     82.00 134.00   0.50    0.50    --  106.20 -61.00 -60.00  104
  8  \w     49.00 127.00   0.50    0.50    --  106.20 -77.00 -60.00  156
  9  \w     94.00 120.00   0.50    0.50    --  106.20  82.00  30.00   52
 10  \w    127.00 194.00   0.50    0.50    --  106.20  82.00  30.00  134
 11  \w     21.00  88.00   0.50    0.50    --  106.20 -45.00  90.00  134
 12  \w     18.00  79.00   0.50    0.50    --  106.20 -61.00 -60.00  122
 13  \w     78.00 122.00   0.50    0.50    --  106.20  45.00  30.00   88
 14  \w     20.00 117.00   0.50    0.50    --  106.20 -30.00 120.00  194
;
_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      0.0667043000
_diffrn_orient_matrix_UB_12      0.0755609000
_diffrn_orient_matrix_UB_13      -0.0350871000
_diffrn_orient_matrix_UB_21      0.2053439000
_diffrn_orient_matrix_UB_22      -0.0178834000
_diffrn_orient_matrix_UB_23      0.0548496000
_diffrn_orient_matrix_UB_31      0.0380825000
_diffrn_orient_matrix_UB_32      -0.0362937000
_diffrn_orient_matrix_UB_33      -0.1005645000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10951
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.457
_diffrn_reflns_theta_min         4.227
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32627
_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    1.670
_exptl_crystal_description       black
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+0.6983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3222
_reflns_number_total             3513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01289k2.cif
_cod_data_source_block           20190516-2
_cod_database_code               7241408
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.89
_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:
 N1(H1A), N2(H2B), C18(H18), C11(H11), C12(H12), C14(H14), C6(H6A), C2(H2A),
 C15(H15)
2.b Idealised tetrahedral OH refined as rotating group:
 O6(H6), O5(H5), O1(H1), O2(H2)
;
_shelx_res_checksum              70890
_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 2.122
_oxdiff_exptl_absorpt_empirical_full_min 0.459