Divalent Silicon-Assisted Activation of Dihydrogen in a Bis(N-heterocyclic silylene)xanthene Nickel(0) Complex for Efficient Catalytic Hydrogenation of Olefins.
Wang, Yuwen; Kostenko, Arseni; Yao, Shenglai; Driess, Matthias; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b07167

data_4126390
_publ_section_title
;
 Divalent Silicon-Assisted Activation of Dihydrogen in a
 Bis(N-heterocyclic silylene)xanthene Nickel(0) Complex for Efficient
 Catalytic Hydrogenation of Olefins.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07167
_journal_year                    2017
_chemical_formula_sum            'C51 H76 N4 Ni O P2 Si2'
_chemical_formula_weight         937.99
_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           'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_cell_angle_alpha                103.260(3)
_cell_angle_beta                 100.102(2)
_cell_angle_gamma                105.877(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2230(3)
_cell_length_b                   12.2612(3)
_cell_length_c                   20.7900(7)
_cell_measurement_reflns_used    11754
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.3330
_cell_measurement_theta_min      3.8930
_cell_volume                     2590.25(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17840
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         3.91
_exptl_absorpt_coefficient_mu    1.860
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         9299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0419P)^2^+0.9470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0823
_reflns_number_gt                8534
_reflns_number_total             9299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b07167_si_002.cif
_cod_data_source_block           Si-Xant-Si-Ni-PMe3-complex-3
_cod_original_cell_volume        2590.25(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4126390