Bis{[amino(iminiumyl)methyl]urea} tetrakis{2-[(dimethylamino)(iminiumyl)methyl]guanidine} di-μ~6~-oxido-tetra-μ~3~-oxido-tetradeca-μ~2~-oxido-octaoxidodecavanadium(V) tetrahydrate
Pérez-Benítez, Aarón; Ariza-Ramírez, Jorge Luis; Fortis-Valera, Monserrat; Arroyo-Carmona, Rosa Elena; Martínez de la Luz, María Isabel; Ramírez-Contreras, Diego; Bernès, Sylvain; IUCrData 7 (2022) x220627–; doi:10.1107/S2414314622006277

data_1567182
_publ_section_title
;
 Bis{[amino(iminiumyl)methyl]urea}
 tetrakis{2-[(dimethylamino)(iminiumyl)methyl]guanidine}
 di-\m~6~-oxido-tetra-\m~3~-oxido-tetradeca-\m~2~-oxido-octaoxidodecavanadium(V)
 tetrahydrate
;
_journal_coeditor_code           WM4167
_journal_issue                   6
_journal_name_full               IUCrData
_journal_page_first              x220627
_journal_paper_doi               10.1107/S2414314622006277
_journal_volume                  7
_journal_year                    2022
_chemical_formula_iupac          '(C4 H12 N5)4 (C2 H7 N4 O)2 [V10 O28], 4H2 O'
_chemical_formula_moiety
'4(C4 H12 N5 +), 2(C2 H7 N4 O +), O28 V10 6-,4(H2 O)'
_chemical_formula_sum            'C20 H70 N28 O34 V10'
_chemical_formula_weight         1756.44
_chemical_name_systematic
;Bis{[amino(iminiumyl)methyl]urea}
tetrakis{2-[(dimethylamino)(iminiumyl)methyl]guanidine}
di-\m~6~-oxido-tetra-\m~3~-oxido-tetradeca-\m~2~-oxido-octaoxidodecavanadium(V) tetrahydrate
;
_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                99.609(3)
_cell_angle_beta                 103.133(3)
_cell_angle_gamma                107.676(3)
_cell_formula_units_Z            1
_cell_length_a                   8.9701(3)
_cell_length_b                   13.2202(5)
_cell_length_c                   14.0861(5)
_cell_measurement_reflns_used    44097
_cell_measurement_temperature    263.0(10)
_cell_measurement_theta_max      30.93
_cell_measurement_theta_min      2.15
_cell_volume                     1499.00(10)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2019)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2019)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2019)
;
_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      263.0(10)
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.997
_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  0.0639
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            66181
_diffrn_reflns_theta_full        19.664
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.415
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_current           0.600
_diffrn_source_power             0.039
_diffrn_source_voltage           65
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>X-AREA</i>; Stoe & Cie, 2019)
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_description       Prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.752
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.828
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     488
_refine_ls_number_reflns         11970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.828
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0523P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                7120
_reflns_number_total             11970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4167sup1.cif
_cod_data_source_block           I
_cod_database_code               1567182
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.936
_shelx_hkl_checksum              10714
_shelx_res_checksum              12687
_cod_database_fobs_code 1567182