Structural, Electrochemical, and Spectroscopic Characterization of a Redox Pair of Sulfite-Based Polyoxotungstates: α-[W18O54(SO3)2]4- and α-[W18O54(SO3)2]5-
Nigel Fay; Alan M. Bond; Carole Baffert; John F. Boas; John R. Pilbrow; De-Liang Long; Leroy Cronin; Inorganic Chemistry 46 (2007) 3502–3510; doi:10.1021/ic062067e

data_4307590
_publ_section_title
;
Structural, Electrochemical, and Spectroscopic Characterization of a Redox
Pair of Sulfite-Based Polyoxotungstates: \a-[W18O54(SO3)2]4- and
\a-[W18O54(SO3)2]5-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3502
_journal_page_last               3510
_journal_paper_doi               10.1021/ic062067e
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '5(C12 H28 N +), (O60 S2 W18 5-), 2(C2 H3 N)'
_chemical_formula_sum            'C64 H146 N7 O60 S2 W18'
_chemical_formula_weight         5347.30
_chemical_name_common            'Compound DL152'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.137(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4863(12)
_cell_length_b                   22.0781(15)
_cell_length_c                   33.587(2)
_cell_measurement_reflns_used    9686
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.74
_cell_measurement_theta_min      2.36
_cell_volume                     12102.1(14)
_computing_cell_refinement       Bruker
_computing_data_collection       Bruker
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker ApexII CCD'
_diffrn_measurement_method       '\w and \p scans'
_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  0.1135
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            132378
_diffrn_reflns_theta_full        20.83
_diffrn_reflns_theta_max         20.83
_diffrn_reflns_theta_min         1.11
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    17.147
_exptl_absorpt_correction_T_max  0.4260
_exptl_absorpt_correction_T_min  0.0864
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.935
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9692
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.68
_refine_diff_density_min         -2.00
_refine_diff_density_rms         0.30
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1086
_refine_ls_number_reflns         12643
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0074P)^2^+1363.9812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                9211
_reflns_number_total             12643
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062067esi20061029_083727.cif
_cod_data_source_block           dl190
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
;
_cod_original_cell_volume        12102.0(15)
_cod_database_code               4307590