Synthesis and crystal structure of 2-amino-3-hydroxypyridinium dioxido(pyridine-2,6-dicarboxylato-κ^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)vanadate(V) and its conversion to nanostructured V~2~O~5~
Hejrani-Dalir, Ali; Tabatabaee, Masumeh; Sheibani, Ali; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229614027983

data_2019774
_publ_section_title
;
 Synthesis and crystal structure of 2-amino-3-hydroxypyridinium
 dioxido(pyridine-2,6-dicarboxylato-\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)vanadate(V)
 and its conversion to nanostructured V~2~O~5~
;
_journal_coeditor_code           WQ3079
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614027983
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '(C5 H7 N2 O) [V (C7 H3 N O4) O2]'
_chemical_formula_moiety         'C7 H3 N O6 V, C5 H7 N2 O'
_chemical_formula_sum            'C12 H10 N3 O7 V'
_chemical_formula_weight         359.17
_chemical_name_systematic
;
2-Amino-3-hydroxypyridinium
dioxido(pyridine-2,6-dicarboxylato-\
\k^2^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)vanadate(V)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.173(3)
_cell_length_b                   6.3586(7)
_cell_length_c                   8.1089(8)
_cell_measurement_reflns_used    4939
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.63
_cell_volume                     1349.5(3)
_computing_cell_refinement
;
APEX2 (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      147(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  'Bruker Triumph'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6889
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.462
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0269P)^2^+1.4082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                1592
_reflns_number_total             1698
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wq3079sup1.cf
_cod_data_source_block           I
_cod_database_code               2019774
_cod_database_fobs_code          2019774