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_7709632
_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 H17 F2 N7 O4 Zn, 2(H2 O)'
_chemical_formula_sum            'C20 H21 F2 N7 O6 Zn'
_chemical_formula_weight         558.81
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-01
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.09.11 svn.r3730fd0d for OlexSys, GUI svn.r6159)
;
_audit_update_record
;
2021-11-26 deposited with the CCDC.	2022-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                105.715(4)
_cell_angle_beta                 95.658(4)
_cell_angle_gamma                110.128(4)
_cell_formula_units_Z            2
_cell_length_a                   9.5983(4)
_cell_length_b                   11.3429(6)
_cell_length_c                   12.5297(6)
_cell_measurement_reflns_used    2590
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.6730
_cell_measurement_theta_min      3.3730
_cell_volume                     1204.87(11)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_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    -24.00  17.00   1.00    4.61    --  -19.31 -99.00 120.00   41
  2  \w     -9.00  89.00   1.00    4.61    --   17.28  37.00 120.00   98
  3  \w     -4.00  86.00   1.00    4.61    --   17.28  57.00 -30.00   90
  4  \w    -52.00  39.00   1.00    4.61    --   17.28 -57.00-180.00   91
;
_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      -0.0208207000
_diffrn_orient_matrix_UB_12      -0.0695630000
_diffrn_orient_matrix_UB_13      -0.0234076000
_diffrn_orient_matrix_UB_21      -0.0195864000
_diffrn_orient_matrix_UB_22      0.0030723000
_diffrn_orient_matrix_UB_23      -0.0549809000
_diffrn_orient_matrix_UB_31      0.0752962000
_diffrn_orient_matrix_UB_32      0.0107361000
_diffrn_orient_matrix_UB_33      -0.0071149000
_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  0.0212
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7161
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         3.065
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.778
_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    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.179
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0337P)^2^+0.4508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3605
_reflns_number_total             4536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04070g2.cif
_cod_data_source_block           Compound_IV
_cod_database_code               7709632
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 F2 N7 O6 Zn'
_reflns_odcompleteness_completeness 99.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N7(H7), C1(H1), C2(H2A), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C18(H18)
;
_shelx_res_checksum              59778
_shelx_hkl_checksum              27144
_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 1.080
_oxdiff_exptl_absorpt_empirical_full_min 0.966