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_7027201
_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         '(C10H12OS4)2 Mo6O19'
_chemical_formula_sum            'C20 H24 Mo6 O21 S8'
_chemical_formula_weight         1432.51
_chemical_name_common            '(Me~3~TTF-CH~2~OH)~2~ Mo~6~O~19~'
_chemical_name_systematic
; 
 ? 
;
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                109.08(2)
_cell_angle_beta                 95.29(2)
_cell_angle_gamma                103.41(2)
_cell_formula_units_Z            1
_cell_length_a                   7.8304(13)
_cell_length_b                   11.288(2)
_cell_length_c                   11.375(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.8
_cell_measurement_theta_min      2.
_cell_volume                     908.7(3)
_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. 2\%'
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9813
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    2.551
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction based on measurments
of equivalent reflections was performed with XPREP
(Siemens-SHELXTL Version 5)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.617
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_obs          0.0260
_refine_ls_shift/esd_max         -0.164
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+1.3641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0797
_refine_ls_wR_factor_obs         0.0669
_reflns_number_observed          3204
_reflns_number_total             3642
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809442jsup1.cif
_cod_data_source_block           adohabs
_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^)+(0.0425P)^2^+1.3641P] 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^)+(0.0425P)^2^+1.3641P] 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        908.8(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027201