Reactivity of Mo(PMe3)6 towards Benzothiophene and Selenophenes: New Pathways Relevant to Hydrodesulfurization
Daniela Buccella; Kevin E. Janak; Gerard Parkin; Journal of the American Chemical Society 130 (2008) 16187–16189; doi:10.1021/ja8070545

data_4108777
_publ_section_title
;
 Reactivity of Mo(PMe3)6 towards Benzothiophene and Selenophenes: New
 Pathways Relevant to Hydrodesulfurization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16187
_journal_page_last               16189
_journal_paper_doi               10.1021/ja8070545
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C45 H106 Mo3 P10 Se2'
_chemical_formula_weight         1402.74
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 112.4780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9949(8)
_cell_length_b                   18.7079(8)
_cell_length_c                   20.3149(9)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      31.26
_cell_measurement_theta_min      2.21
_cell_volume                     6319.4(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      125(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            53895
_diffrn_reflns_theta_full        32.54
_diffrn_reflns_theta_max         32.54
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    2.019
_exptl_absorpt_correction_T_max  0.8551
_exptl_absorpt_correction_T_min  0.7516
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.178(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         21432
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0613
_reflns_number_gt                18157
_reflns_number_total             21432
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8070545_si_008.cif
_cod_data_source_block           semos20
_cod_database_code               4108777