Electron Transfer-Oxygen Transfer Oxygenation of Sulfides Catalyzed by the H5PV2Mo10O40 Polyoxometalate
Alexander M. Khenkin; Gregory Leitus; Ronny Neumann; Journal of the American Chemical Society 132 (2010) 11446–11448; doi:10.1021/ja105183w

data_4102939
_publ_section_title
;
 Electron Transfer-Oxygen Transfer Oxygenation of Sulfides Catalyzed by
 the H5PV2Mo10O40 Polyoxometalate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11446
_journal_page_last               11448
_journal_paper_doi               10.1021/ja105183w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'2(Mo12 O40 P), 2(C18 H43 N O5 S4 V), C8 H20 O6 S2 V, C2 H3 N, O2'
_chemical_formula_sum            'C46 H109 Mo24 N3 O98 P2 S10 V3'
_chemical_formula_weight         5110.28
_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                103.03(4)
_cell_angle_beta                 94.58(3)
_cell_angle_gamma                93.89(3)
_cell_formula_units_Z            1
_cell_length_a                   12.713(3)
_cell_length_b                   14.020(3)
_cell_length_c                   20.454(4)
_cell_measurement_reflns_used    105354
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      1.7
_cell_volume                     3526.6(15)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Apex2'
_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      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker KappaApexII CCD'
_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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            92173
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    2.512
_exptl_absorpt_correction_T_max  0.9062
_exptl_absorpt_correction_T_min  0.8243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Apex2'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2457
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.390
_refine_diff_density_min         -4.120
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1212
_refine_ls_number_reflns         19728
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0776
_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^)+(0.0364P)^2^+52.2808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1793
_reflns_number_gt                15717
_reflns_number_total             19728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105183w_si_002.cif
_cod_data_source_block           n295
_cod_original_cell_volume        3526.6(14)
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4102939