Anodic oxidation of molybdenum and tungsten in alcohols: isolation and X-ray single-crystal study of side products
Kessler, Vadim G.; Panov, Andrei N.; Turova, Nataliya Ya.; Starikova, Zoya A.; Yanovsky, Alexandr I.; Dolgushin, Fedor M.; Pisarevsky, Alexandr P.; Struchkov, Yuri T.; Journal of the Chemical Society, Dalton Transactions  (1998) 21–; doi:10.1039/a704198e

data_7028023
_publ_section_title
;
 Anodic oxidation of molybdenum and tungsten in alcohols: isolation and
 X-ray single-crystal study of side products
;
_journal_issue                   1
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              21
_journal_paper_doi               10.1039/a704198e
_journal_year                    1998
_chemical_formula_moiety         'C30 H74 Li4 O24 W2 ++, O19 W6 --'
_chemical_formula_sum            'C30 H74 Li4 O43 W8'
_chemical_formula_weight         2621.5
_chemical_name_systematic
;
Tetralithium-hexakis(2-methoxyethoxy)-tetrakis(2-
-methoxyethanol)-tetraoxo-di-tungsten  hexawolframate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                89.90(3)
_cell_angle_beta                 110.73(3)
_cell_angle_gamma                103.01(3)
_cell_formula_units_Z            1
_cell_length_a                   11.461(5)
_cell_length_b                   11.828(4)
_cell_length_c                   12.623(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      11
_cell_volume                     1553.6(11)
_computing_cell_refinement       'CAD4 Enraf-Nonius'
_computing_data_collection       'CAD4 Enraf-Nonius'
_computing_data_reduction        'SHELXTL PLUS 5 (gamma version)'
_computing_molecular_graphics    'SHELXTL PLUS 5 (gamma version)'
_computing_publication_material  'SHELXTL PLUS 5 (gamma version)'
_computing_structure_refinement  'SHELXTL PLUS 5 (gamma version)'
_computing_structure_solution    'SHELXTL PLUS 5 (gamma version)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4 Enraf-Nonius'
_diffrn_measurement_method       'CAD4 Enraf-Nonius'
_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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8628
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    14.843
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.246
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_F_000             1202
_refine_diff_density_max         7.705
_refine_diff_density_min         -5.568
_refine_diff_density_rms         0.448
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.976
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_obs          0.0591
_refine_ls_shift/esd_max         -0.011
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1761
_refine_ls_wR_factor_obs         0.1594
_reflns_number_observed          5988
_reflns_number_total             8230
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            e704198sup1.cif
_cod_data_source_block           str_VII
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.1360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7028023