Water-soluble copper(II) 5-fluorouracil complexes bearing polypyridyl co-ligands: Synthesis, structures and anticancer activity
Icsel, Ceyda; Yilmaz, Veysel T.; Aygün, Muhittin; Erkisa, Merve; Ulukaya, Engin; Dalton Transactions  (2023) –; doi:10.1039/D3DT00363A

data_7712560
_publ_section_title
;
 Water-soluble copper(II) 5-fluorouracil complexes bearing polypyridyl
 co-ligands: Synthesis, structures and anticancer activity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00363A
_journal_year                    2023
_chemical_formula_moiety         'C19 H13 Cl Cu F N5 O2'
_chemical_formula_sum            'C19 H13 Cl Cu F N5 O2'
_chemical_formula_weight         461.33
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-17
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.09.11 svn.r3730fd0d for OlexSys, GUI svn.r6159)
;
_audit_update_record
;
2022-03-12 deposited with the CCDC.	2023-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.472(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6071(9)
_cell_length_b                   13.0317(14)
_cell_length_c                   12.3107(11)
_cell_measurement_reflns_used    2403
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.0360
_cell_measurement_theta_min      3.8400
_cell_volume                     1861.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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      5.00  49.00   1.00   10.10    --   20.23 -99.00  90.00   44
  2  \w    -21.00  11.00   1.00   10.10    --  -22.26 -99.00 -30.00   32
  3  \w    -20.00  21.00   1.00   10.10    --  -22.26 -99.00-180.00   41
  4  \w    -95.00  20.00   1.00   10.10    --  -22.26   0.00   0.00  115
;
_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      -0.0196027000
_diffrn_orient_matrix_UB_12      -0.0325403000
_diffrn_orient_matrix_UB_13      -0.0428423000
_diffrn_orient_matrix_UB_21      -0.0320613000
_diffrn_orient_matrix_UB_22      0.0412717000
_diffrn_orient_matrix_UB_23      -0.0230796000
_diffrn_orient_matrix_UB_31      0.0481716000
_diffrn_orient_matrix_UB_32      0.0142783000
_diffrn_orient_matrix_UB_33      -0.0308781000
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7139
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.126
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.354
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.367
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0449P)^2^+0.2973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1142
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2856
_reflns_number_total             3800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00363a2.cif
_cod_data_source_block           Compound_V
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7712560
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C19 H13 Cl Cu F N5 O2'
_shelx_estimated_absorpt_t_max   0.695
_shelx_estimated_absorpt_t_min   0.594
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 N2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C19(H19)
;
_shelx_res_checksum              54663
_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 1.123
_oxdiff_exptl_absorpt_empirical_full_min 0.886