Copper(ii) complexes with tridentate halogen-substituted Schiff base ligands: synthesis, crystal structures and investigating the effect of halogenation, leaving groups and ligand flexibility on antiproliferative activities.
Kordestani, Nazanin; Amiri Rudbari, Hadi; Fernandes, Alexandra R.; Raposo, Luís R; Luz, André; Baptista, Pedro V.; Bruno, Giuseppe; Scopelliti, Rosario; Fateminia, Zohreh; Micale, Nicola; Tumanov, Nikolay; Wouters, Johan; Abbasi Kajani, Abolghasem; Bordbar, Abdol-Khalegh; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3990–4007; doi:10.1039/d0dt03962d

data_7706631
_publ_section_title
;
 Copper(ii) complexes with tridentate halogen-substituted Schiff base
 ligands: synthesis, crystal structures and investigating the effect of
 halogenation, leaving groups and ligand flexibility on antiproliferative
 activities.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3990
_journal_page_last               4007
_journal_paper_doi               10.1039/d0dt03962d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C14 H11 Br2 Cu N3 O4'
_chemical_formula_sum            'C14 H11 Br2 Cu N3 O4'
_chemical_formula_weight         508.61
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-10-08 deposited with the CCDC.	2021-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3364(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.25361(14)
_cell_length_b                   10.15411(9)
_cell_length_c                   21.8598(2)
_cell_measurement_reflns_used    14237
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.2040
_cell_measurement_theta_min      4.7800
_cell_volume                     3163.77(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury 3.10.3 (CCDC, 2018)'
_computing_publication_material  'CIFTab (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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    -63.00  22.00   1.00    1.00    --  -43.01  57.00  90.00   85
  2  \w    -84.00  30.00   1.00    1.00    --  -43.01  19.00  30.00  114
  3  \w      2.00  55.00   1.00    1.00    --   43.01 -99.00-180.00   53
  4  \w     30.00  98.00   1.00    1.00    --   43.01-125.00 -60.00   68
  5  \w     38.00 141.00   1.00    4.00    --  109.26 -77.00 -60.00  103
  6  \w    108.00 141.00   1.00    4.00    --  109.26 -77.00  90.00   33
  7  \w    109.00 138.00   1.00    4.00    --  109.26 -30.00  90.00   29
  8  \w     85.00 177.00   1.00    4.00    --  109.26  45.00 120.00   92
  9  \w    107.00 146.00   1.00    4.00    --  109.26 111.00  60.00   39
 10  \w    109.00 177.00   1.00    4.00    --  109.26 111.00  30.00   68
 11  \w    137.00 164.00   1.00    4.00    --  109.26  30.00-150.00   27
 12  \w    100.00 136.00   1.00    4.00    --  109.26  30.00-150.00   36
 13  \w     37.00 138.00   1.00    4.00    --  109.26 -30.00 -60.00  101
 14  \w     79.00 115.00   1.00    4.00    --  109.26-111.00  90.00   36
 15  \w     51.00 100.00   1.00    4.00    --  109.26 -94.00 150.00   49
 16  \w     33.00  86.00   1.00    4.00    --  109.26 -30.00  90.00   53
 17  \w     33.00  79.00   1.00    4.00    --  109.26 -77.00  90.00   46
 18  \w     49.00 116.00   1.00    4.00    --  109.26-111.00 -90.00   67
 19  \w   -123.00 -89.00   1.00    1.00    --  -43.01 -99.00  90.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22226
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.303
_diffrn_reflns_theta_min         3.692
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.110
_exptl_absorpt_correction_T_max  0.469
_exptl_absorpt_correction_T_min  0.110
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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            purple
_exptl_crystal_density_diffrn    2.136
_exptl_crystal_description       prism
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.533
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.00118(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0396P)^2^+2.5995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6275
_reflns_number_total             6440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03962d2.cif
_cod_data_source_block           Cu(Br2-L1)NO3
_cod_depositor_comments
;
Adding full bibliography for 7706630--7706633.cif.

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_moiety     'C28 H22 Br4 Cu2 N6 O8'
_cod_original_formula_sum        'C28 H22 Br4 Cu2 N6 O8'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1017.23
_cod_database_code               7706631
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.098
_shelx_estimated_absorpt_t_max   0.396
_shelx_res_checksum              9036
_shelx_hkl_checksum              37838
_publcif_funding_html
;
;