(Et~4~N)~4~[V~4~O~12~]·2H~2~O
Nakano, Hiroyuki; Ozeki, Tomoji; Yagasaki, Atsushi; Acta Crystallographica Section C 58 (2002) m464–m465; doi:10.1107/S0108270102013008

data_2012944
_publ_section_title
;
 (Et~4~N)~4~[V~4~O~12~]&#x00B7;2H~2~O
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m464
_journal_page_last               m465
_journal_paper_doi               10.1107/S0108270102013008
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C8 H20 N)4 [V4 O12] , 2H2 O'
_chemical_formula_moiety         '4(C8 H20 N) 1+ , O12 V4 4- , 2(H2 O)'
_chemical_formula_structural     '(C8 H20 N)4 [V4 O12] , 2H2 O'
_chemical_formula_sum            'C32 H84 N4 O14 V4'
_chemical_formula_weight         952.79
_chemical_name_common
;
Tetrakis(tetraethylammonium) cyclotetravanadate dihydrate
;
_chemical_name_systematic
;
Tetrakis(tetraethylammonium) cyclo-tetra-\m-oxo-tetrakis[dioxovanadium(V)]
dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.8360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0187(3)
_cell_length_b                   10.5729(2)
_cell_length_c                   16.0212(4)
_cell_measurement_reflns_used    4000
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      1.00
_cell_volume                     2305.73(9)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku Ultrax-18 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.114
_diffrn_reflns_av_sigmaI/netI    0.135
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22145
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.87
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         7001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.125
_refine_ls_R_factor_gt           0.058
_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^)+(0.0673P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.120
_refine_ls_wR_factor_ref         0.141
_reflns_number_gt                3962
_reflns_number_total             7001
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob1072.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2305.70(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2012944
_cod_database_fobs_code          2012944