An efficient one-pot synthesis of pyrazole complexes formed in situ: synthesis, crystal structure, Hirshfeld surface analysis and in vitro biological properties.
Adach, Anna; Tyszka-Czochara, Małgorzata; Daszkiewicz, Marek; Acta crystallographica. Section C, Structural chemistry 79 (2023) 520–529; doi:10.1107/S2053229623010021

data_2312364
_publ_section_title
;
 An efficient one-pot synthesis of pyrazole complexes formed in situ:
 synthesis, crystal structure, Hirshfeld surface analysis and in vitro
 biological properties.
;
_journal_coeditor_code           DG3048
_journal_issue                   12
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              520
_journal_page_last               529
_journal_paper_doi               10.1107/S2053229623010021
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac
'[Co0.20 Zn1.80 Br1.40 Cl0.60 (C5 H7 N2)2 (C5 H8 N2)2]'
_chemical_formula_moiety         'C20 H30 Br1.40 Cl0.60 Co0.20 N8 Zn1.80'
_chemical_formula_sum            'C20 H30 Br1.4 Cl0.6 Co0.2 N8 Zn1.8'
_chemical_formula_weight         645.11
_chemical_name_systematic
Bis(\m-3,5-dimethyl-1<i>H</i>-pyrazole)-\k^2^<i>N</i>^1^:<i>N</i>^2^;\k^2^<i>N</i>^2^:<i>N</i>^1^-bis[bromido/chlorido(0.7/0.3)bis(3,5-dimethyl-1<i>H</i>-pyrazole-\k<i>N</i>^1^)cobalt/zinc(0.1/0.9)]
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                84.826(2)
_cell_angle_beta                 69.156(2)
_cell_angle_gamma                87.133(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2698(2)
_cell_length_b                   8.4060(2)
_cell_length_c                   10.3062(2)
_cell_measurement_reflns_used    8024
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.1550
_cell_measurement_theta_min      3.4800
_cell_volume                     666.70(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.6249
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Rigaku Xcalibur diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0144
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15822
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.433
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.924
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2020)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       prism
_exptl_crystal_F_000             325
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.2264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                2608
_reflns_number_total             3035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dg3048sup1.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C20 H30 Br1.40 Cl0.60 Co0.20 N8 Zn1.80'
_cod_database_code               2312364
_shelx_estimated_absorpt_t_min   0.440
_shelx_estimated_absorpt_t_max   0.555
_shelx_hkl_checksum              6217
_shelx_res_checksum              90629
_cod_database_fobs_code 2312364