Tetraammonium bis(metforminium) di-μ~6~-oxido-tetra-μ~3~-oxido-tetradeca-μ~2~-oxido-octaoxidodecavanadium(V) hexahydrate
Polito-Lucas, J. Alberto; Núñez-Ávila, José A.; Bernès, Sylvain; Pérez-Benítez, Aarón; IUCrData 6 (2021) x210634–; doi:10.1107/S2414314621006349

data_1563716
_publ_section_title
;
 Tetraammonium bis(metforminium)
 di-\m~6~-oxido-tetra-\m~3~-oxido-tetradeca-\m~2~-oxido-octaoxidodecavanadium(V)
 hexahydrate
;
_journal_coeditor_code           IM4012
_journal_issue                   6
_journal_name_full               IUCrData
_journal_page_first              x210634
_journal_paper_doi               10.1107/S2414314621006349
_journal_volume                  6
_journal_year                    2021
_chemical_formula_iupac          '(N H4)4 (C4 H12 N5)2 [V10 O28], 6H2 O'
_chemical_formula_moiety
'4(H4 N +), 2(C4 H12 N5 +), O28 V10 6-, 6(H2 O)'
_chemical_formula_sum            'C8 H52 N14 O34 V10'
_chemical_formula_weight         1398.03
_chemical_name_systematic
;
Tetraammonium bis(metforminium)
di-\m~6~-oxido-tetra-\m~3~-oxido-tetradeca-\m~2~-oxido-octaoxidodecavanadium(V)
hexahydrate
;
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                81.081(2)
_cell_angle_beta                 70.906(2)
_cell_angle_gamma                63.321(2)
_cell_formula_units_Z            1
_cell_length_a                   9.7965(2)
_cell_length_b                   10.1010(2)
_cell_length_c                   13.0974(3)
_cell_measurement_reflns_used    131899
_cell_measurement_temperature    295.0(10)
_cell_measurement_theta_max      33.67
_cell_measurement_theta_min      2.19
_cell_volume                     1094.30(5)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2020)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2020)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2020)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      295.0(10)
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            94693
_diffrn_reflns_theta_full        19.664
_diffrn_reflns_theta_max         28.500
_diffrn_reflns_theta_min         2.194
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_current           0.55
_diffrn_source_power             0.03575
_diffrn_source_voltage           65
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_T_max  0.9067
_exptl_absorpt_correction_T_min  0.4261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-AREA; Stoe & Cie, 2020)
;
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_description       tetrahedron
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.189
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.951
_refine_ls_extinction_coef       0.0048(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     361
_refine_ls_number_reflns         11269
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.0305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                9224
_reflns_number_total             11269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            im4012sup1.cif
_cod_data_source_block           I
_cod_database_code               1563716
_shelx_estimated_absorpt_t_min   0.760
_shelx_estimated_absorpt_t_max   0.819
_shelx_hkl_checksum              59916
_shelx_res_checksum              55702
_cod_database_fobs_code 1563716