Tetrakis(tetramethylammonium) Dihydrogendecavanadate Acetic Acid 2.8-Hydrate, [N(CH~3~)~4~]~4~[H~2~V~10~O~28~].CH~3~COOH.2.8H~2~O
Pecquenard, Brigitte; Zavalij, Peter Y.; Whittingham, M. Stanley; Acta Crystallographica Section C 54 (1998) 1833–1835; doi:10.1107/S0108270198009044

data_2007876
_publ_section_title
;
 Tetrakis(tetramethylammonium) Dihydrogendecavanadate Acetic Acid
 2.8-Hydrate, [N(CH~3~)~4~]~4~[H~2~V~10~O~28~].CH~3~COOH.2.8H~2~O
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1833
_journal_page_last               1835
_journal_paper_doi               10.1107/S0108270198009044
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac
'(C4 H12 N)4 [H2 V10 O28] , C2 H4 O2 , 2.8H2 O'
_chemical_formula_sum            'C18 H59.6 N4 O32.8 V10'
_chemical_formula_weight         1366.6
_chemical_name_systematic
;
tetrakis-tetramethylammonium dihydrogen-decavanadate acetic acid hydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                73.0920(10)
_cell_angle_beta                 78.8750(10)
_cell_angle_gamma                78.8490(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6690(4)
_cell_length_b                   12.6905(4)
_cell_length_c                   15.8223(5)
_cell_measurement_reflns_used    2012
_cell_measurement_temperature    295
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     2362.48(13)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'PLATON97, PLUTON97 (Spek, 1990)'
_computing_publication_material  CSD
_computing_structure_refinement  CSD
_computing_structure_solution    'CSD (Akselrud et al, 1993)'
_diffrn_ambient_temperature      295
_diffrn_measurement_device       'Siemens Smart CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_av_sigmaI/netI    0.025
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14948
_diffrn_reflns_theta_max         28.5
_diffrn_reflns_theta_min         2
_diffrn_standards_decay_%        0.8
_exptl_absorpt_coefficient_mu    1.98
_exptl_absorpt_correction_T_max  0.563
_exptl_absorpt_correction_T_min  0.511
_exptl_absorpt_correction_type   'multi-scan SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          .36
_exptl_crystal_size_mid          .32
_exptl_crystal_size_min          .29
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.82
_refine_ls_hydrogen_treatment    H_atoms:_see_text
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     609
_refine_ls_number_reflns         9335
_refine_ls_R_factor_obs          0.046
_refine_ls_shift/esd_max         0.01
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F~o~) + 0.002F~o~^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.071
_reflns_number_observed          9335
_reflns_number_total             10265
_reflns_observed_criterion       'F~o~ > 4\s(F~o~)'
_cod_data_source_file            bk1385.cif
_cod_data_source_block           bk1385
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/[\s^2^(F~o~) + 0.002F~o~^2^]'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w = 1/[\s^2^(F~o~) +
0.002F~o~^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2362.5(3)
_cod_original_formula_sum        'C18 H59.6 N4 V10 O32.8'
_cod_database_code               2007876