Crystal structure of bis[4-(dimethylamino)pyridinium] aquabis(oxalato)oxidovanadate(IV) dihydrate
Sehimi, Hiba; Chérif, Ichraf; Zid, Mohamed Faouzi; Acta Crystallographica Section E 72 (2016) 1002–1005; doi:10.1107/S2056989016009695

data_2241732
_publ_section_title
;
 Crystal structure of bis[4-(dimethylamino)pyridinium]
 aquabis(oxalato)oxidovanadate(IV) dihydrate
;
_journal_coeditor_code           WM5298
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1002
_journal_page_last               1005
_journal_paper_doi               10.1107/S2056989016009695
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '(C7 H11 N2)2 [V (C2 O4)2 O (H2 O)], 2H2 O'
_chemical_formula_moiety         '2(C7 H11 N2 +), C4 H2 O10 V 2-, 2(H2 O)'
_chemical_formula_sum            'C18 H28 N4 O12 V'
_chemical_formula_weight         543.38
_chemical_name_systematic
;
Bis[4-(dimethylamino)pyridinium] aquabis(oxalato)oxidovanadate(IV) dihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.197(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.682(2)
_cell_length_b                   7.689(4)
_cell_length_c                   21.280(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2383.4(13)
_computing_cell_refinement
;
CAD-4 EXPRESS (Duisenberg, 1992)
;
_computing_data_collection
;
CAD-4 EXPRESS (Duisenberg, 1992)
;
_computing_data_reduction
;
XCAD4 (Harms & Wocadlo, 1995)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            4165
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.968
_diffrn_reflns_theta_min         2.797
_diffrn_standards_decay_%        1.4
_diffrn_standards_interval_count 120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.9079
_exptl_absorpt_correction_T_min  0.8411
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North <i>et al.</i>, 1968)
;
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.257
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2599
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0482P)^2^+1.2556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1064
_reflns_number_gt                1850
_reflns_number_total             2599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5298sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2383.3(13)
_cod_database_code               2241732
_cod_database_fobs_code          2241732
_shelx_hkl_checksum              92334
_shelx_res_checksum              67832