Organotin Derivatives of α-[XIIIW9O33]9- (X = As, Sb) Heteropolytungstates. Solution- and Solid-State Characterization of [{(C6H5Sn)2O}2H(α-AsW9O33)2]9- and [(C6H5Sn)3Na3(α-SbW9O33)2]6-
Gerta Sazani; Michael H. Dickman; Michael T. Pope; Inorganic Chemistry 39 (2000) 939–943; doi:10.1021/ic991095c

data_4300195
_publ_section_title
;
Organotin Derivatives of \a-[XIIIW9O33]9- (X = As, Sb) Heteropolytungstates.
Solution- and Solid-State Characterization of
[{(C6H5Sn)2O}2H(\a-AsW9O33)2]9- and [(C6H5Sn)3Na3(\a-SbW9O33)2]6-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              939
_journal_page_last               943
_journal_paper_doi               10.1021/ic991095c
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C24 As2 Na4 O93.88 Sn4 W18'
_chemical_formula_weight         5816.18
_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-97
_cell_angle_alpha                93.59(3)
_cell_angle_beta                 106.187(19)
_cell_angle_gamma                112.23(3)
_cell_formula_units_Z            1
_cell_length_a                   15.272(6)
_cell_length_b                   15.303(6)
_cell_length_c                   16.760(7)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.53
_cell_measurement_theta_min      5.07
_cell_volume                     3419(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device_type  'serial detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9859
_diffrn_reflns_theta_max         24.86
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    16.363
_exptl_absorpt_correction_T_max  0.00903
_exptl_absorpt_correction_T_min  0.00049
_exptl_absorpt_correction_type   'semi-empirical from psi scans'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.825
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2537
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .40
_refine_diff_density_max         4.382
_refine_diff_density_min         -2.285
_refine_diff_density_rms         0.630
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         8655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.1062
_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^)+(0.2000P)^2^+140.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3060
_refine_ls_wR_factor_ref         0.3187
_reflns_number_gt                7544
_reflns_number_total             8655
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        3419(2)
_cod_database_code               4300195