Novel 5-fluorouracil complexes of Zn(II) with pyridine-based ligands as potential anticancer agents
Icsel, Ceyda; Yilmaz, Veysel T.; Aygün, Muhittin; Erkisa, merve; Ulukaya, Engin; Dalton Transactions  (2022) –; doi:10.1039/D1DT04070G

data_7709633
_publ_section_title
;
 Novel 5-fluorouracil complexes of Zn(II) with pyridine-based ligands as
 potential anticancer agents
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04070G
_journal_year                    2022
_chemical_formula_moiety         'C20 H12 F2 N6 O4 Zn'
_chemical_formula_sum            'C20 H12 F2 N6 O4 Zn'
_chemical_formula_weight         503.73
_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             2022-02-04
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.09.11 svn.r3730fd0d for OlexSys, GUI svn.r6159)
;
_audit_update_record
;
2022-02-05 deposited with the CCDC.	2022-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                81.183(19)
_cell_angle_beta                 73.210(19)
_cell_angle_gamma                67.59(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9142(19)
_cell_length_b                   8.956(2)
_cell_length_c                   13.328(3)
_cell_measurement_reflns_used    779
_cell_measurement_temperature    228(2)
_cell_measurement_theta_max      23.3170
_cell_measurement_theta_min      3.3340
_cell_volume                     940.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      228(60)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -81.00  -1.00   1.00   55.84    --  -16.23 -57.00-120.00   80
  2  \w    -25.00  21.00   1.00   55.84    --  -16.23 -99.00 150.00   46
  3  \w    -35.00  50.00   1.00   55.84    --  -16.23  77.00  90.00   85
  4  \w    -85.00  10.00   1.00   55.84    --  -16.23 -19.00 -60.00   95

There is no relevant diffraction at 50 degree in 2 theta,
the required minimum resolution has not been reached.
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0809619000
_diffrn_orient_matrix_UB_12      -0.0208989000
_diffrn_orient_matrix_UB_13      -0.0350445000
_diffrn_orient_matrix_UB_21      0.0322900000
_diffrn_orient_matrix_UB_22      -0.0621285000
_diffrn_orient_matrix_UB_23      0.0363619000
_diffrn_orient_matrix_UB_31      -0.0177229000
_diffrn_orient_matrix_UB_32      -0.0553208000
_diffrn_orient_matrix_UB_33      -0.0233908000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.1586
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5757
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.848
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.371
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       prism
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1502
_refine_ls_R_factor_gt           0.0738
_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^)+(0.0305P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1834
_reflns_number_total             3319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04070g2.cif
_cod_data_source_block           Compound_II
_cod_database_code               7709633
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H12 F2 N6 O4 Zn'
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.831
_reflns_odcompleteness_completeness 99.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N6(H6), C1(H1), C2(H2), C3(H3), C5(H5), C6(H6A), C8(H8), C9(H9),
 C10(H10), C14(H14), C18(H18)
;
_shelx_res_checksum              57550
_shelx_hkl_checksum              92839
_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 2.932
_oxdiff_exptl_absorpt_empirical_full_min 0.827