Hexakis(2-aminopyridinium) di-μ~6~-oxido-tetra-μ~3~-oxido-tetradeca-μ~2~-oxido-octaoxidodecavanadium(V) dihydrate
Yuan, Caixia; Lu, Liping; Zhu, Miaoli; Ma, Qi; Wu, Yanbo; Acta Crystallographica Section E 65 (2009) m267–m268; doi:10.1107/S1600536809004334

data_2221073
_publ_section_title
;Hexakis(2-aminopyridinium)
 di-\m~6~-oxido-tetra-\m~3~-oxido-tetradeca-\m~2~-oxido-octaoxidodecavanadium(V)
 dihydrate
;
_journal_coeditor_code           HB2897
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m267
_journal_page_last               m268
_journal_paper_doi               10.1107/S1600536809004334
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '(C5 H7 N2)6 [V10 O28], 2H2 O'
_chemical_formula_moiety         '6(C5 H7 N2 +), O28 V10 6-, 2(H2 O)'
_chemical_formula_sum            'C30 H46 N12 O30 V10'
_chemical_formula_weight         1564.19
_chemical_name_systematic
;
Hexakis(2-aminopyridinium) di-\m~6~-oxido-tetra-\m~3~-oxido-
tetradeca-\m~2~-oxido-octaoxidodecavanadium(V) dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 97.416(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.840(3)
_cell_length_b                   18.180(6)
_cell_length_c                   14.299(5)
_cell_measurement_reflns_used    3889
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.24
_cell_volume                     2536.6(14)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL/PC (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART 1K 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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9858
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.860
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.446
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.293
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.293
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0095P)^2^+8.6635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1280
_reflns_number_gt                3949
_reflns_number_total             4341
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2897.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2221073
_cod_database_fobs_code          2221073