Nickel Hydrides Supported by a Non-Innocent Diphosphine Arene Pincer: Mechanistic Studies of Nickel-Arene H-Migration and Partial Arene Hydrogenation
Sibo Lin; Michael W. Day; Theodor Agapie; Journal of the American Chemical Society 133 (2011) 3828–3831; doi:10.1021/ja200368y

data_4105808
_publ_section_title
;
 Nickel Hydrides Supported by a Non-Innocent Diphosphine Arene Pincer:
 Mechanistic Studies of Nickel-Arene H-Migration and Partial Arene
 Hydrogenation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3828
_journal_page_last               3831
_journal_paper_doi               10.1021/ja200368y
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
'C30 H41 Ni P2, C32 H44 N Ni P2, 2(C F3 O3 S)'
_chemical_formula_sum            'C32 H42.5 F3 N0.5 Ni O3 P2 S'
_chemical_formula_weight         691.88
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.212(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.7671(12)
_cell_length_b                   12.6722(6)
_cell_length_c                   20.3587(9)
_cell_measurement_reflns_used    9110
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.24
_cell_volume                     6632.0(5)
_computing_cell_refinement       'Bruker SAINT-Plus v7.66A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.66A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 9 settings'
_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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            156014
_diffrn_reflns_theta_full        30.57
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.8511
_exptl_absorpt_correction_T_min  0.8324
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       Block
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.634
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.908
_refine_ls_hydrogen_treatment    Unrestrained
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     1143
_refine_ls_number_reflns         20232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.908
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.1001
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                16091
_reflns_number_total             20232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200368y_si_004.cif
_cod_data_source_block           sbl16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Difference Fourier map' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_formula_sum        'C32 H42.50 F3 N0.50 Ni O3 P2 S'
_cod_database_code               4105808