Relative basicities of the oxygen atoms of the Linquist polyoxometalate [Mo6O19]2− and their recognition by hydroxyl groups in radical cation salts based on functionalized tetrathiafulvalene π donors
Dolbecq, Anne; Guirauden, Aude; Fourmigué, Marc; Boubekeur, Kamal; Batail, Patrick; Rohmer, Marie-Madeleine; Bénard, Marc; Coulon, Claude; Sallé, Marc; Blanchard, Philippe; Journal of the Chemical Society, Dalton Transactions  (1999) 1241–; doi:10.1039/a809442j

data_7027202
_publ_section_title
;
 Relative basicities of the oxygen atoms of the Linquist polyoxometalate
 [Mo6O19]2&#x2212; and their recognition by hydroxyl groups in radical
 cation salts based on functionalized tetrathiafulvalene \p donors
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1241
_journal_paper_doi               10.1039/a809442j
_journal_year                    1999
_chemical_formula_moiety         '(C10 H10 O2 S6)2 Mo6 O19'
_chemical_formula_sum            'C20 H20 Mo6 O23 S12'
_chemical_formula_weight         1588.72
_chemical_name_systematic
;
Bis[3,4-(ethylenedithio)-3'-4'-bis(hydroxymethyl)-tetrathiafulvalene]
nonadecaoxohexamolybdate(VI)
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.342(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.654(2)
_cell_length_b                   11.5411(8)
_cell_length_c                   17.1100(12)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.8
_cell_measurement_theta_min      2.0
_cell_volume                     3998.9(6)
_computing_cell_refinement       'SELECT (Stoe IPDS)'
_computing_data_collection       'EXPOSE (Stoe IPDS)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'rotation, phi incr. 1.1\%'
_diffrn_radiation_detector       'area detector'
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34134
_diffrn_reflns_theta_max         26.87
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.538
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT (Stoe IPDS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.639
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.767
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.292
_refine_ls_goodness_of_fit_obs   1.376
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         8120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.306
_refine_ls_restrained_S_obs      1.376
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_obs          0.0637
_refine_ls_shift/esd_max         0.012
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+82.1288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1335
_refine_ls_wR_factor_obs         0.1292
_reflns_number_observed          6918
_reflns_number_total             8121
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809442jsup1.cif
_cod_data_source_block           adoh2
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+82.1288P] 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^)+(0.0176P)^2^+82.1288P] 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        3998.8(5)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7027202