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_1565689
_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         'C32 H30 Br2 Cu2 N4 O6, 2(N O3)'
_chemical_formula_sum            'C32 H30 Br2 Cu2 N6 O12'
_chemical_formula_weight         977.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 106.503(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4084(14)
_cell_length_b                   14.848(2)
_cell_length_c                   13.645(2)
_cell_measurement_reflns_used    7090
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.30
_cell_measurement_theta_min      2.26
_cell_volume                     1827.6(5)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0436
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20020
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         2.07
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.420
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3756
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0455P)^2^+1.7622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                2964
_reflns_number_total             3756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2020-499-119186.cif
_cod_data_source_block           728
_cod_database_code               1565689
_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
 O3-H3
 0.85 with sigma of 0.01
 C15-H3
 1.86254 with sigma of 0.02
 Cu1-H3
 2.780739 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C5(H5), C10(H10), C12(H12), C3(H3A), C2(H2), C1(H1A), C13(H13),
 C4(H4), C15(H15), C8(H8)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_olex2_submission_special_instructions 'No special instructions were received'