Three-Coordinate NiII: Tracing the Origin of an Unusual, Facile Si-C(sp3) Bond Cleavage in [(tBu2PCH2SiMe2)2N]Ni+
Benjamin C. Fullmer; Hongjun Fan; Maren Pink; John C. Huffman; Nikolay P. Tsvetkov; Kenneth G. Caulton; Journal of the American Chemical Society 133 (2011) 2571–2582; doi:10.1021/ja108426f

data_4105674
_publ_contact_author             'J.C. Huffman'
_publ_section_title
;
 Three-Coordinate NiII: Tracing the Origin of an Unusual, Facile Si-C(sp3)
 Bond Cleavage in [(tBu2PCH2SiMe2)2N]Ni+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2571
_journal_page_last               2582
_journal_paper_doi               10.1021/ja108426f
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C23 H52 F3 N Ni O3 P2 S Si2'
_chemical_formula_sum            'C23 H52 F3 N Ni O3 P2 S Si2'
_chemical_formula_weight         656.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_date             05/18/2007
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.1300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5700(6)
_cell_length_b                   17.0742(8)
_cell_length_c                   17.1530(9)
_cell_measurement_reflns_used    2020
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.92
_cell_volume                     3286.0(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'Reciprocal Net (http://recipnet.org)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
'   0.30 degree frames measured for 20.16 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w 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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32834
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0307P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0570
_reflns_number_gt                6335
_reflns_number_total             7544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja108426f_si_002.cif
_cod_data_source_block           07078
_cod_original_sg_symbol_Hall     '-P 2yn   '
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4105674