Mechanistic Insights on the Hydrodesulfurization of Biphenyl-2-thiol with Nickel Compounds
Jorge Torres-Nieto; William W. Brennessel; William D. Jones; Juventino J. García; Journal of the American Chemical Society 131 (2009) 4120–4126; doi:10.1021/ja809457s

data_4104073
_publ_section_title
;
 Mechanistic Insights on the Hydrodesulfurization of Biphenyl-2-thiol with
 Nickel Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4120
_journal_page_last               4126
_journal_paper_doi               10.1021/ja809457s
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C38 H50 Ni P2 S2'
_chemical_formula_sum            'C38 H50 Ni P2 S2'
_chemical_formula_weight         691.55
_chemical_name_common            jonjt03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   30.896(4)
_cell_length_b                   50.891(7)
_cell_length_c                   9.0942(13)
_cell_measurement_reflns_used    3985
_cell_measurement_temperature    105.0(1)
_cell_measurement_theta_max      32.47
_cell_measurement_theta_min      2.63
_cell_volume                     14299(3)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      105.0(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0837
_diffrn_reflns_av_sigmaI/netI    0.0887
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       75
_diffrn_reflns_limit_k_min       -76
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            47236
_diffrn_reflns_theta_full        32.58
_diffrn_reflns_theta_max         32.58
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.9550
_exptl_absorpt_correction_T_min  0.8861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5888
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
'Flack H D (1983), 6018 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         12856
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+1.1638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                9768
_reflns_number_total             12856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809457s_si_002_2.cif
_cod_data_source_block           jonjt03
_cod_database_code               4104073