Arrested 1,2-Hydrogen Migration from Silicon to Nickel upon Oxidation of a Three-Coordinate Ni(I) Silyl Complex
Vlad M. Iluc; Gregory L. Hillhouse; Journal of the American Chemical Society 132 (2010) 11890–11892; doi:10.1021/ja1052329

data_4102970
_publ_contact_author_address
;Gordon Center for Integrative Sciences E419B
Department of Chemistry
The University of chicago
929 East 57th Street
Chicago, IL, 60637
;
_publ_contact_author_email       g-hillhouse@uchicago.edu
_publ_contact_author_fax         773-702-0805
_publ_contact_author_name        'Gregory L. Hillhouse'
_publ_contact_author_phone       773-702-7057
_publ_section_title
;
 Arrested 1,2-Hydrogen Migration from Silicon to Nickel upon Oxidation of
 a Three-Coordinate Ni(I) Silyl Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11890
_journal_page_last               11892
_journal_paper_doi               10.1021/ja1052329
_journal_volume                  132
_journal_year                    2010
_chemical_compound_source        synthetic
_chemical_formula_moiety         'C36 H63 Ni P2 Si'
_chemical_formula_sum            'C36 H63 Ni P2 Si'
_chemical_formula_weight         644.60
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.061(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6888(8)
_cell_length_b                   18.7901(17)
_cell_length_c                   22.348(2)
_cell_measurement_reflns_used    124
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      1.83
_cell_volume                     3628.2(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22250
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.83
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.9604
_exptl_absorpt_correction_T_min  0.8651
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_recrystallization_method 'hexanes, -35C'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         8466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+3.6677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                6814
_reflns_number_total             8466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1052329_si_002_2.cif
_cod_data_source_block           vlad06m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4102970