First 12-tungstovanadate Keggin compound: synthesis and crystal structure of [Me4N]7[VW12O40]·15H2O
Khan, M. Ishaque; Cevik, Sabri; Hayashi, Randy; Journal of the Chemical Society, Dalton Transactions  (1999) 1651–; doi:10.1039/a808760a

data_7702361
_publ_section_title
;
 First 12-tungstovanadate Keggin compound: synthesis and crystal structure
 of [Me4N]7[VW12O40]&#x00B7;15H2O
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1651
_journal_paper_doi               10.1039/a808760a
_journal_year                    1999
_chemical_formula_moiety         '7(C4 H12 N)+ (V W12 O40)7- 15(H2 O)'
_chemical_formula_structural     '7(C4 H12 N)+ (V W12 O40)7- 15(H2 O)'
_chemical_formula_sum            'C28 H114 N7 O55 V W12'
_chemical_formula_weight         3686.40
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.302(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9094(2)
_cell_length_b                   20.8420(6)
_cell_length_c                   15.1180(2)
_cell_measurement_reflns_used    6390
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     4002.04(14)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       'phi scan frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19354
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0.04
_diffrn_standards_number         602
_exptl_absorpt_coefficient_mu    17.377
_exptl_absorpt_correction_T_max  0.121
_exptl_absorpt_correction_T_min  0.072
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'opaque prism'
_exptl_crystal_F_000             3364
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.759
_refine_diff_density_min         -5.204
_refine_diff_density_rms         0.359
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_obs          0.0439
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+52.2021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1271
_refine_ls_wR_factor_obs         0.1157
_reflns_number_observed          7841
_reflns_number_total             9710
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808760a.txt
_cod_data_source_block           97278
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+52.2021P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. A new data item '_refine_ls_weighting_details'
was created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+52.2021P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P21/m
_cod_database_code               7702361