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_4300194
_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            'C18 H83 Na6 O102.5 Sb2 Sn3 W18'
_chemical_formula_weight         5986.65
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.933(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7952(1)
_cell_length_b                   22.3133(2)
_cell_length_c                   34.4393(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      1.09
_cell_volume                     10599.58(14)
_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_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            116732
_diffrn_reflns_theta_full        28.57
_diffrn_reflns_theta_max         28.57
_diffrn_reflns_theta_min         1.09
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    20.780
_exptl_absorpt_correction_T_max  0.363
_exptl_absorpt_correction_T_min  0.0075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             10644
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.34
_refine_diff_density_max         4.874
_refine_diff_density_min         -3.958
_refine_diff_density_rms         0.534
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         25977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0901
_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^)+(0.0246P)^2^+740.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1573
_reflns_number_gt                21318
_reflns_number_total             25977
_reflns_threshold_expression     >2sigma(I)
_cod_original_formula_sum        'C18 H83 Na6 O102.50 Sb2 Sn3 W18'
_cod_database_code               4300194