Oxygen/Sulfur Substitution Reactions of Tetraoxometalates Effected by Electrophilic Carbon and Silicon Reagents
David V. Partyka; R. H. Holm; Inorganic Chemistry 43 (2004) 8609–8616; doi:10.1021/ic040097g

data_4312195
_publ_section_title
;
 Oxygen/Sulfur Substitution Reactions of Tetraoxometalates Effected by
 Electrophilic Carbon and Silicon Reagents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8609
_journal_page_last               8616
_journal_paper_doi               10.1021/ic040097g
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C22 H44 Mo N2 O3 S2'
_chemical_formula_weight         544.65
_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                104.87(3)
_cell_angle_beta                 95.78(3)
_cell_angle_gamma                116.56(3)
_cell_formula_units_Z            2
_cell_length_a                   9.815(2)
_cell_length_b                   10.689(2)
_cell_length_c                   15.045(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1321.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8883
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.678
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         6178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+0.1739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                4876
_reflns_number_total             6178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040097g_2.cif
_cod_data_source_block           tri1a
_cod_original_cell_volume        1321.7(5)
_cod_database_code               4312195