Crystal structure of bis(ammonium) bis[pentaaqua(dimethylformamide)zinc(II)] decavanadate tetrahydrate
Ebrahimi, Arash; Gyepes, Róbert; Bujdoš, Marek; Krivosudský, Lukáš; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022003449

data_2244068
_publ_section_title
;
 Crystal structure of bis(ammonium)
 bis[pentaaqua(dimethylformamide)zinc(II)] decavanadate tetrahydrate
;
_journal_coeditor_code           YZ2017
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022003449
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac
'(N H4)2 [Zn (C3 H7 N O) (H2 O1)5]2 [V10 O28], 4H2 O'
_chemical_formula_moiety
'2(H4 N +), 2(C3 H17 N O6 Zn 2+), O28 V10 6-, 4(H2 O)'
_chemical_formula_sum            'C6 H50 N4 O44 V10 Zn2'
_chemical_formula_weight         1522.64
_chemical_name_systematic
;
Bis(ammonium) bis[pentaaqua(dimethylformamide)zinc(II)]
decavanadate tetrahydrate
;
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 108.6280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.5436(6)
_cell_length_b                   8.6538(4)
_cell_length_c                   16.7362(7)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5185
_cell_measurement_theta_min      2.5685
_cell_volume                     2133.27(16)
_computing_cell_refinement
;
SAINT (Bruker, 2019)
;
_computing_data_collection
;
<i>Instrument Service</i> (Bruker, 2021)
;
_computing_data_reduction
;
SAINT (Bruker, 2019)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD with Buker APEXII detector'
_diffrn_measurement_method       'data from phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         2.167
_exptl_absorpt_coefficient_mu    3.312
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.370
_exptl_crystal_description       prism
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.489
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.623
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4901
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0284P)^2^+1.1852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                4354
_reflns_number_total             4901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yz2017sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2244068
_shelx_estimated_absorpt_t_min   0.294
_shelx_estimated_absorpt_t_max   0.733
_shelx_hkl_checksum              83485
_shelx_res_checksum              18218
_cod_database_fobs_code 2244068