Synthesis and structure of pentakis(2-aminopyridinium) nonavanado(V)tellurate(VI)
Mrad, Houda; Maalaoui, Ahlem; Rzaigui, Mohamed; Akriche, Samah; Acta Crystallographica Section E Crystallographic Communications 80 (2024) –; doi:10.1107/S2056989024010533

data_2023305
_publ_section_title
;
 Synthesis and structure of pentakis(2-aminopyridinium)
 nonavanado(V)tellurate(VI)
;
_journal_coeditor_code           HB8109
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024010533
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '(C5 H7 N2)5 [Te V9 O28]'
_chemical_formula_moiety         '5(C5 H7 N2 +), O28 Te V9 5-'
_chemical_formula_structural     'Te V9 O28, (C5 H7 N2)5'
_chemical_formula_sum            'C25 H35 N10 O28 Te V9'
_chemical_formula_weight         1509.69
_chemical_name_systematic
;
Pentakis(2-aminopyridinium) nonavanado(V)tellurate(VI)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 122.530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.661(2)
_cell_length_b                   23.251(2)
_cell_length_c                   19.602(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9
_cell_volume                     4480.9(12)
_computing_cell_refinement
;
CAD-4 Express (Enraf--Nonius, 1994)
;
_computing_data_collection
;
CAD-4 Express (Enraf--Nonius, 1994)
;
_computing_data_reduction
;
XCAD4 (Harms & Wocadlo, 1996)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
WinGX publication routines (Farrugia, 2012) and <i>CrystalExplorer</i>
(Wolff et al., 2012)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.1042
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25752
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         27.986
_diffrn_reflns_theta_min         2.064
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        -2
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.312
_exptl_absorpt_correction_T_max  0.8067
_exptl_absorpt_correction_T_min  0.7445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_description       prism
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.191
_refine_diff_density_min         -1.743
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         21889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1818
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+23.7680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.2112
_reflns_number_gt                10265
_reflns_number_total             21889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8109.cif
_cod_data_source_block           I
_cod_original_cell_volume        4481.1(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2023305
_shelx_hkl_checksum              66245
_shelx_res_checksum              13073
_shelxl_version_number           .2013