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_4312198
_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            'C8 H20 N O3 Re S'
_chemical_formula_weight         396.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.38(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.1330(14)
_cell_length_b                   21.366(4)
_cell_length_c                   16.628(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2533.4(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17047
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    9.743
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_refine_diff_density_max         5.606
_refine_diff_density_min         -11.499
_refine_diff_density_rms         0.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         6210
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0968
_refine_ls_shift/su_max          0.114
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+169.4513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1864
_refine_ls_wR_factor_ref         0.1911
_reflns_number_gt                5192
_reflns_number_total             6210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040097g_6.cif
_cod_data_source_block           mono1a
_cod_original_cell_volume        2533.5(9)
_cod_database_code               4312198