Room-Temperature Desulfurization of Dibenzothiophene Mediated by [(i-Pr2PCH2)2NiH]2
David A. Vicic; William D. Jones; Journal of the American Chemical Society 119 (1997) 10855–10856; doi:10.1021/ja972544f

data_4117060
_publ_section_title
;
 Room-Temperature Desulfurization of Dibenzothiophene Mediated by
 [(i-Pr2PCH2)2NiH]2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10855
_journal_page_last               10856
_journal_paper_doi               10.1021/ja972544f
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C28 H65 F6 Ni2 P5 S'
_chemical_formula_weight         820.13
_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
_cell_angle_alpha                118.5080(10)
_cell_angle_beta                 92.7060(10)
_cell_angle_gamma                104.8550(10)
_cell_formula_units_Z            4
_cell_length_a                   16.34770(10)
_cell_length_b                   16.6742(2)
_cell_length_c                   17.21450(10)
_cell_measurement_temperature    193(2)
_cell_volume                     3905.41(8)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens SMART'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18127
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    NA
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         12160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_obs          0.0558
_refine_ls_shift/esd_max         0.180
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+9.3513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1297
_refine_ls_wR_factor_obs         0.1176
_reflns_number_observed          8893
_reflns_number_total             12178
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja972544f_2.cif
_cod_data_source_block           sad_[(dippe)2Ni2(H)(S)]PF6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NA' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+9.3513P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+9.3513P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3905.40(6)
_cod_database_code               4117060