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_4102969
_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_formula_sum            'C148 H170 B2 F48 Ni2 O3 P4 Si2'
_chemical_formula_weight         3227.90
_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-97
_cell_angle_alpha                94.4880(10)
_cell_angle_beta                 108.7170(10)
_cell_angle_gamma                106.8960(10)
_cell_formula_units_Z            1
_cell_length_a                   14.5285(9)
_cell_length_b                   16.1699(10)
_cell_length_c                   18.5044(11)
_cell_measurement_reflns_used    192
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      2.35
_cell_volume                     3868.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17607
_diffrn_reflns_theta_full        25.27
_diffrn_reflns_theta_max         25.27
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.9603
_exptl_absorpt_correction_T_min  0.8505
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Norton et. al 1968'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         14050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0911P)^2^+11.5389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2227
_reflns_number_gt                9627
_reflns_number_total             14050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1052329_si_002_1.cif
_cod_data_source_block           vlad04m
_cod_database_code               4102969