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_7712563
_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
'C28 H18 Cu F N6 O2, C4 H2 F N2 O2, H2 O, 3[H2O]'
_chemical_formula_sum            'C32 H28 Cu F2 N8 O8'
_chemical_formula_weight         700.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_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
;
2023-03-06 deposited with the CCDC.	2023-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.728(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.1277(13)
_cell_length_b                   19.623(3)
_cell_length_c                   24.848(3)
_cell_measurement_reflns_used    1986
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.9000
_cell_measurement_theta_min      3.3710
_cell_volume                     6369.0(14)
_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_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_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    -31.00  79.00   1.00   10.18    --   20.07   0.00 150.00  110
  2  \w    -30.00  11.00   1.00   10.18    --  -22.10 -77.00-180.00   41
  3  \w   -103.00 -54.00   1.00   10.18    --  -22.10 168.00  -1.31   49
;
_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  0.0670
_diffrn_reflns_av_unetI/netI     0.1215
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9494
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.296
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.836
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       prism
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5577
_refine_ls_number_restraints     414
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1655
_refine_ls_R_factor_gt           0.1103
_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^)+(0.0861P)^2^+79.0813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2640
_refine_ls_wR_factor_ref         0.2998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3029
_reflns_number_total             5577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00363a2.cif
_cod_data_source_block           Compound_II
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7712563
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.817
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3.a Riding coordinates:
 N7(H7)
3.b Free rotating group:
 O1W(H1WA,H1WB)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H2), C2(H2A), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28),
  C29(H29), C30(H70), C8(H8)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 246 electrons were 
found in a volume of 762\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[H2O] per Asymmetric Unit 
which account for 240 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              55382
_shelx_fab_checksum              57808
_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
;