Hexakis[3-(aminocarbonyl)pyridinium] decavanadate(V) dihydrate
Pacigová, Silvia; Rakovský, Erik; Sivák, Michal; Žák, Zdirad; Acta Crystallographica Section C 63 (2007) m419–m422; doi:10.1107/S0108270107028557

data_2016133
_publ_section_title
;
 Hexakis[3-(aminocarbonyl)pyridinium] decavanadate(V) dihydrate
;
_journal_coeditor_code           DN3044
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m419
_journal_page_last               m422
_journal_paper_doi               10.1107/S0108270107028557
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C6 H7 N2 O)6 [V10 O28], 2H2 O'
_chemical_formula_moiety         '6(C6 H7 N2 O +), V10 O28 6-, 2(H2 O)'
_chemical_formula_sum            'C36 H46 N12 O36 V10'
_chemical_formula_weight         1732.25
_chemical_name_common
;
1-H-nicotinamidium(1+) decavanadate(V) dihydrate
;
_chemical_name_systematic
;
Hexakis[3-(aminocarbonyl)pyridinium] decavanadate(V) dihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.60(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.806(9)
_cell_length_b                   9.5460(13)
_cell_length_c                   23.577(10)
_cell_measurement_reflns_used    24882
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3.0
_cell_volume                     5566(3)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics
;
PLATON (Spek, 2003) and DIAMOND (Brandenburg, 2007)
;
_computing_publication_material
;
SHELXL97, DIAMOND and publCIF (Westrip, 2007)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 0.06
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Kuma KM-4 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0115
_diffrn_reflns_av_sigmaI/netI    0.0097
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34597
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_exptl_absorpt_coefficient_mu    1.714
_exptl_absorpt_correction_T_max  0.7831
_exptl_absorpt_correction_T_min  0.4812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.506
_refine_ls_extinction_coef       0.00011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         5811
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0341P)^2^+8.29P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0624
_reflns_number_gt                5173
_reflns_number_total             5811
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn3044.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2016133
_cod_database_fobs_code          2016133