All-Inorganic Networks and Tetramer Based on Tin(II)-Containing Polyoxometalates: Tuning Structural and Spectral Properties with Lone-Pairs.
Zhao, Chongchao; Glass, Elliot N.; Chica, Bryant; Musaev, Djamaladdin G.; Sumliner, Jordan M.; Dyer, R. Brian; Lian, Tianquan; Hill, Craig L.; Journal of the American Chemical Society 136 (2014) 12085–; doi:10.1021/ja5060127

data_4122428
_publ_section_title
;
 All-Inorganic Networks and Tetramer Based on Tin(II)-Containing
 Polyoxometalates: Tuning Structural and Spectral Properties with
 Lone-Pairs.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12085
_journal_paper_doi               10.1021/ja5060127
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'Na9 O77.50 Sb2 Sn6 W18'
_chemical_formula_sum            'Na9 O77.5 Sb2 Sn6 W18'
_chemical_formula_weight         5711.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.778(3)
_cell_length_b                   17.778(3)
_cell_length_c                   45.221(13)
_cell_measurement_reflns_used    1881
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.23
_cell_volume                     12378(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1171
_diffrn_reflns_av_sigmaI/netI    0.0873
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12880
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    27.546
_exptl_absorpt_correction_T_max  0.5546
_exptl_absorpt_correction_T_min  0.2124
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   xprep
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             14718
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.056
_refine_diff_density_max         5.875
_refine_diff_density_min         -4.457
_refine_diff_density_rms         0.691
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1841
_refine_ls_wR_factor_ref         0.2252
_reflns_number_gt                1923
_reflns_number_total             3350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5060127_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4122426--4122428.cif.'
_cod_original_sg_symbol_H-M      R-3m
_cod_original_formula_sum        'Na9 O77.50 Sb2 Sn6 W18'
_cod_database_code               4122428