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_7028022
_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         'C8 H25 Li1 Mo2 O10'
_chemical_formula_sum            'C8 H25 Li Mo2 O10'
_chemical_formula_weight         480.10
_chemical_name_systematic
;
Lithium-heptamethoxy-methanol-dioxo-di-molybdenum(v)
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.33(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.449(2)
_cell_length_b                   14.256(3)
_cell_length_c                   14.223(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.5
_cell_measurement_theta_min      13.5
_cell_volume                     1699.1(7)
_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 verion)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       '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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5049
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_F_000             960
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.238
_refine_ls_goodness_of_fit_obs   1.374
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.299
_refine_ls_restrained_S_obs      1.374
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_obs          0.0337
_refine_ls_shift/esd_max         0.186
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+2.4710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1030
_refine_ls_wR_factor_obs         0.0886
_reflns_number_observed          3058
_reflns_number_total             4509
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            e704198sup1.cif
_cod_data_source_block           str_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 2.4.2 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^)+(0.0357P)^2^+2.4710P] 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^)+(0.0357P)^2^+2.4710P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1699.1(6)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C8 H25 Li1 Mo2 O10'
_cod_database_code               7028022