Perchlorate-induced structural diversity in thiosemicarbazone copper(ii) complexes provides insights to understand the reactivity in acidic and basic media
Gil-García, Rubén; Madariaga, Gotzon; Jiménez-Pérez, Alondra; Herrán-Torres, Ignacio; Gago-González, Adrián; Ugalde, María; Januskaitis, Vaidas; Barrera-García, Joaquín; Insausti, Maite; S. Galletero, María; Borrás, Joaquín; Cuevas, José Vicente; Pedrido, Rosa; Gómez-Saiz, Patricia; Lezama, Luis; García-Tojal, Javier; CrystEngComm 25 (2023) 2213–2226; doi:10.1039/D3CE00119A

data_7246401
_publ_section_title
;
 Perchlorate-induced structural diversity in thiosemicarbazone copper(ii)
 complexes provides insights to understand the reactivity in acidic and
 basic media
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2213
_journal_page_last               2226
_journal_paper_doi               10.1039/D3CE00119A
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         '2(C7 H10 Cl2 Cu N4 O9 S), H2 O'
_chemical_formula_sum            'C14 H22 Cl4 Cu2 N8 O19 S2'
_chemical_formula_weight         939.39
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-11-05T09:19:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2022-11-04 deposited with the CCDC.	2023-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.29(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.429(6)
_cell_length_b                   18.170(13)
_cell_length_c                   13.688(5)
_cell_measurement_reflns_used    1038
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      52.1
_cell_measurement_theta_min      3.3
_cell_volume                     3160(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'STOE Stadivari'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1135
_diffrn_reflns_av_unetI/netI     0.118
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12025
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         26.195
_diffrn_reflns_theta_min         2.028
_exptl_absorpt_coefficient_mu    1.909
_exptl_absorpt_correction_T_max  0.8369
_exptl_absorpt_correction_T_min  0.7131
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        a grid of 32 x 32 x 32 = 32768 sampling points was used
;
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_description       'Irregular shape described by 15 faces'
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         2879
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      0.87
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                1453
_reflns_number_total             2879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00119a2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7246399--7246403.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7246401