Synthesis, X-ray structures, and magnetic properties of seven polynuclear Cu(ii) complexes containing pyrazole-3,5-dicarboxylate with various ancillary ligands
Klongdee, Fatima; Sasada, Yuto; Nakano, Motohiro; Chainok, Kittipong; Youngme, Sujittra; Boonmak, Jaursup; New Journal of Chemistry 47 (2023) 9669–9680; doi:10.1039/D3NJ00821E

data_7062432
_publ_section_title
;
 Synthesis, X-ray structures, and magnetic properties of seven polynuclear
 Cu(ii) complexes containing pyrazole-3,5-dicarboxylate with various
 ancillary ligands
;
_journal_issue                   20
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9669
_journal_page_last               9680
_journal_paper_doi               10.1039/D3NJ00821E
_journal_volume                  47
_journal_year                    2023
_chemical_formula_sum            'C32 H20 Cu4 N16 Na4 O18'
_chemical_formula_weight         1262.76
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-04-18 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.90320(10)
_cell_length_b                   11.90320(10)
_cell_length_c                   41.3061(7)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.8285
_cell_measurement_theta_min      2.6135
_cell_volume                     5852.50(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       BrukerAPEX2
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            3109
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.730
_diffrn_reflns_theta_min         3.122
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    1.535
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.107
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3109
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0588
_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^)+(0.1093P)^2^+17.2151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.1926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2466
_reflns_number_total             3109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00821e2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7062429--7062435.cif.'
_cod_original_cell_volume        5852.50(14)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7062432
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.790
_shelx_estimated_absorpt_t_max   1.550
_shelx_res_checksum              22865