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_4104072
_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         'C40 H74 Ni2 P4 S'
_chemical_formula_sum            'C40 H74 Ni2 P4 S'
_chemical_formula_weight         828.35
_chemical_name_common            jonjt01
_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                 110.827(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.369(3)
_cell_length_b                   10.9191(15)
_cell_length_c                   19.087(3)
_cell_measurement_reflns_used    3948
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      31.85
_cell_measurement_theta_min      2.22
_cell_volume                     4357.4(11)
_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      100.0(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            77743
_diffrn_reflns_theta_full        32.57
_diffrn_reflns_theta_max         32.57
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  0.8122
_exptl_absorpt_correction_T_min  0.7657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.771
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         15799
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0394P)^2^+2.6521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                10710
_reflns_number_total             15799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809457s_si_002_1.cif
_cod_data_source_block           jonjt01
_cod_original_cell_volume        4357.4(10)
_cod_database_code               4104072