Binuclear Schiff base copper(II) complexes: Syntheses, crystal structures, HSA interaction and anti-cancer properties
Jiang, Shengshi; Ni, Honghui; Liu, Fen; Gu, Shanshan; Yu, Ping; Gou, Yi; Inorganica Chimica Acta 499 (2020) 119186–; doi:10.1016/j.ica.2019.119186

data_1565687
_publ_section_title
;
 Binuclear Schiff base copper(II) complexes: Syntheses, crystal
 structures, HSA interaction and anti-cancer properties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119186
_journal_paper_doi               10.1016/j.ica.2019.119186
_journal_volume                  499
_journal_year                    2020
_chemical_formula_moiety         'C29 H24 Cu2 F2 N5 O8, N O3'
_chemical_formula_sum            'C29 H24 Cu2 F2 N6 O11'
_chemical_formula_weight         797.62
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                66.540(10)
_cell_angle_beta                 66.118(10)
_cell_angle_gamma                66.799(9)
_cell_formula_units_Z            1
_cell_length_a                   9.253(7)
_cell_length_b                   9.338(7)
_cell_length_c                   11.101(9)
_cell_measurement_reflns_used    4986
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.47
_cell_volume                     773.0(10)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7939
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.09
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.460
_exptl_absorpt_correction_T_max  0.9047
_exptl_absorpt_correction_T_min  0.6366
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         2823
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1152P)^2^+0.7821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1598
_reflns_number_gt                2554
_reflns_number_total             2823
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2020-499-119186.cif
_cod_data_source_block           732b
_cod_database_code               1565687
_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 C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O8-N4
 1.25 with sigma of 0.02
 O3-N3
 1.25 with sigma of 0.02
 O6-N4
 1.25 with sigma of 0.02
 O9-H9
 0.85 with sigma of 0.01
 C15-H9
 1.930174 with sigma of 0.02
 Cu1-H9
 2.821844 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim
Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Others
 Fixed Sof: O3(0.5) O4(0.5) O5(0.5) O6(0.5) O7(0.5) O8(0.5) O9(0.5) H9(0.5)
 N3(0.5) N4(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C12(H12),
 C13(H13)
5.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;