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_7712559
_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         '2(C24 H20 Cu F N8 O2), 2(N O3), 5(H2 O)'
_chemical_formula_sum            'C48 H50 Cu2 F2 N18 O15'
_chemical_formula_weight         1284.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-12-23
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.09.11 svn.r3730fd0d for OlexSys, GUI svn.r6159)
;
_audit_update_record
;
2022-12-24 deposited with the CCDC.	2023-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.091(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.6860(11)
_cell_length_b                   9.7121(9)
_cell_length_c                   18.3253(18)
_cell_measurement_reflns_used    1724
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      22.8770
_cell_measurement_theta_min      3.7810
_cell_volume                     2707.7(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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      292(2)
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  39.00   1.00    5.00    --   14.20  77.00  60.00   37
  2  \w    -37.00  37.00   1.00    5.00    --   14.20 -77.00-150.00   74
  3  \w    -46.00  29.00   1.00    5.00    --   14.20 -19.00  60.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_unetI/netI     0.2357
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8982
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.039
_diffrn_reflns_theta_max         25.039
_diffrn_reflns_theta_min         3.107
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.854
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.706
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         4614
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.709
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0146P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1736
_reflns_number_total             4614
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 6.2171\% 
around [0.99 0.06 0.14] (reciprocal) or [0.95 0.14 0.29] (direct)
;
_cod_data_source_file            d3dt00363a2.cif
_cod_data_source_block           Compound_III
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               7712559
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.670
_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,H) groups
2. Restrained distances
 O5-N9 \\sim O4-N9 \\sim O3B-N9 \\sim O3A-N9
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C4, O2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1, O1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N2, C4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N2, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C22, C23
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(O3A)=1-FVAR(1)
 Sof(O3B)=FVAR(1)
 Fixed Sof: H1WA(0.5) H1WB(0.5)
5.a Free rotating group:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB), O2W(H2WA,H2WB)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H2), N4(H4), N7(H7), C3(H3), C5(H5), C6(H6), C7(H7A), C8(H8), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21),
  C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              85434
_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
;