Copper(II) and zinc(II) complexes with Hydrazone: Synthesis, crystal structure, Hirshfeld surface and antibacterial activity
Santiago, Pedro H.O.; Santiago, Mariana B.; Martins, Carlos H.G.; Gatto, Claudia C.; Inorganica Chimica Acta 508 (2020) 119632–; doi:10.1016/j.ica.2020.119632

data_1564509
_publ_section_title
;
 Copper(II) and zinc(II) complexes with Hydrazone: Synthesis, crystal
 structure, Hirshfeld surface and antibacterial activity
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119632
_journal_paper_doi               10.1016/j.ica.2020.119632
_journal_volume                  508
_journal_year                    2020
_chemical_formula_moiety         'C13 H12 Br2 Cu N4 O, 2(H2 O)'
_chemical_formula_sum            'C13 H16 Br2 Cu N4 O3'
_chemical_formula_weight         499.66
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                95.985(2)
_cell_angle_beta                 97.046(2)
_cell_angle_gamma                119.341(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8985(11)
_cell_length_b                   8.9337(11)
_cell_length_c                   12.8937(16)
_cell_measurement_reflns_used    3651
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      22.70
_cell_measurement_theta_min      2.65
_cell_volume                     870.61(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0838
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20209
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.491
_diffrn_reflns_theta_min         1.621
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.861
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1739 before and 0.0922 after correction.
The Ratio of minimum to maximum transmission is 0.6816.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_description       Block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.286
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0013(5)
_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   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0178P)^2^+0.1596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2384
_reflns_number_total             3219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-508-119632.cif
_cod_data_source_block           ccg_phs_cu10_0m
_cod_database_code               1564509
_shelx_estimated_absorpt_t_max   0.285
_shelx_estimated_absorpt_t_min   0.197
_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
2. Restrained distances
3.a Free rotating group:
 H2A(O2,H2B,H3A,O3,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C10(H10), C1(H1), C4(H4A), C13(H13), C2(H2), C11(H11), C3(H3), C12(H12)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              1972
_shelx_hkl_checksum              53694