A tris-oxovanadium pyrogallate complex: synthesis, structure, and magnetic and electronic properties
Mkhadder, Hassan; Denis, Morgane; Giménez-Marqués, Mónica; Cañón-Mancisidor, Walter; Humbert, Bernard; Deunf, Elise; Poizot, Philippe; Devic, Thomas; Dalton Transactions  (2021) –; doi:10.1039/D1DT01990B

data_7708175
_publ_section_title
;
 A tris-oxovanadium pyrogallate complex: synthesis, structure, and
 magnetic and electronic properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01990B
_journal_year                    2021
_chemical_formula_moiety         C24H23K3N2O14V3
_chemical_formula_sum            'C24 H23 K3 N2 O14 V3'
_chemical_formula_weight         833.57
_chemical_name_common            K3V3O3(pgal)3.2DMF
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-07-28 deposited with the CCDC.	2021-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.210(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1630(3)
_cell_length_b                   26.1908(8)
_cell_length_c                   15.0823(4)
_cell_measurement_reflns_used    5561
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      2.5730
_cell_volume                     3125.87(18)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2006)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SHELXS-86
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2930
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67173
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34565
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        23.768
_diffrn_reflns_theta_max         26.604
_diffrn_reflns_theta_min         2.568
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.142
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89567
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_description       prism
_exptl_crystal_F_000             1676
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0418P)^2^+1.6024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5309
_reflns_number_total             7285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01990b2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7708175
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              55610