Cation Controlled Assembly and Transformation of Mono- and Bi-Sulfite Templated Dawson-Type Polyoxotungstates
Jun Yan; De-Liang Long; Haralampos N. Miras; Leroy Cronin; Inorganic Chemistry 49 (2010) 1819–1825; doi:10.1021/ic9021646

data_4314850
_publ_section_title
;
 Cation Controlled Assembly and Transformation of Mono- and Bi-Sulfite
 Templated Dawson-Type Polyoxotungstates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1819
_journal_page_last               1825
_journal_paper_doi               10.1021/ic9021646
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         '6(C6 H16 N O3 +), (H2 O60 S1 W18 6-)'
_chemical_formula_sum            'C36 H98 N6 O78 S W18'
_chemical_formula_weight         5204.56
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.971(1)
_cell_angle_beta                 76.702(2)
_cell_angle_gamma                82.723(2)
_cell_formula_units_Z            1
_cell_length_a                   13.4468(3)
_cell_length_b                   13.9726(4)
_cell_length_c                   14.3083(4)
_cell_measurement_reflns_used    24829
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      1.51
_cell_volume                     2349.88(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'WinGX, (Farrugia, 1999)'
_computing_publication_material  'WinGX, (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Nonius Kappa CCD'
_diffrn_measurement_method       '\w 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  0.0823
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34817
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    22.063
_exptl_absorpt_correction_T_max  0.2713
_exptl_absorpt_correction_T_min  0.0959
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
  P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst.
   (1965), 18, 1035-1038
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.678
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.18
_refine_diff_density_min         -2.93
_refine_diff_density_rms         0.33
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         9225
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+31.3589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                7457
_reflns_number_total             9225
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic9021646_si_002_1.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

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_database_code               4314850