Carbon-Sulfur Bond Cleavage and Hydrodesulfurization of Thiophenes by Tungsten
Aaron Sattler; Gerard Parkin; Journal of the American Chemical Society 133 (2011) 3748–3751; doi:10.1021/ja111034g

data_4105781
_publ_section_title
;
 Carbon-Sulfur Bond Cleavage and Hydrodesulfurization of Thiophenes by
 Tungsten
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3748
_journal_page_last               3751
_journal_paper_doi               10.1021/ja111034g
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C20 H48 P4 S W'
_chemical_formula_weight         628.37
_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                85.772(2)
_cell_angle_beta                 72.371(2)
_cell_angle_gamma                68.5870(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6343(11)
_cell_length_b                   12.1821(14)
_cell_length_c                   13.5960(15)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      30.62
_cell_measurement_theta_min      2.34
_cell_volume                     1414.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22975
_diffrn_reflns_theta_full        30.63
_diffrn_reflns_theta_max         30.63
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    4.387
_exptl_absorpt_correction_T_max  0.8440
_exptl_absorpt_correction_T_min  0.5056
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         8664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0197P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0508
_reflns_number_gt                7815
_reflns_number_total             8664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja111034g_si_002_5.cif
_cod_data_source_block           wsphs10
_cod_database_code               4105781