Synthesis and structural study of tris(2,6-diaminopyridinium) bis(oxalato)dioxidovanadate(V) 2.5-hydrate
Sehimi, Hiba; Akitsu, Takashiro; Zid, Mohamed Faouzi; Acta Crystallographica Section E 75 (2019) 680–684; doi:10.1107/S2056989019005267

data_2242918
_publ_section_title
;
 Synthesis and structural study of tris(2,6-diaminopyridinium)
 bis(oxalato)dioxidovanadate(V) 2.5-hydrate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              680
_journal_page_last               684
_journal_paper_doi               10.1107/S2056989019005267
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '(C5 H8 N3)3 [V O2 (C2 O4)2], 2.5H2 O'
_chemical_formula_moiety         '3(C5 H8 N3 +), C4 O10 V 3-, 2.5(H2 O)'
_chemical_formula_sum            'C19 H29 N9 O12.5 V'
_chemical_formula_weight         634.45
_chemical_name_systematic
;
Tris(2,6-diaminopyridinium) bis(oxalato)dioxidovanadate(V) 2.5-hydrate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 116.551(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.972(2)
_cell_length_b                   7.5746(4)
_cell_length_c                   20.8208(12)
_cell_measurement_reflns_used    33946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.586
_cell_measurement_theta_min      2.187
_cell_volume                     5498.0(5)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32414
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.586
_diffrn_reflns_theta_min         2.187
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.92924
_exptl_absorpt_correction_T_min  0.87714
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            Orange-brown
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.541
_exptl_crystal_size_mid          0.307
_exptl_crystal_size_min          0.276
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.662
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         8409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0395P)^2^+5.9089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                7884
_reflns_number_total             8409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vn2145sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-09-17
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '6(C5 H8 N3 +), 2(C4 O10 V 3-), 5(H2 O)'
_cod_original_formula_sum        'C38 H58 N18 O25 V2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1268.90
_cod_database_code               2242918
_cod_database_fobs_code          2242918
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.888
_shelx_hkl_checksum              76221
_shelx_res_checksum              88752