Mild Protocol for the Synthesis of Stable Nickel Complexes Having Primary and Secondary Silyl Ligands
Adhikari, Debashis; Pink, Maren; Mindiola, Daniel J.; Organometallics 28 (2009) 2072–; doi:10.1021/om801187b

data_4068976
_publ_section_title
;
 Mild Protocol for the Synthesis of Stable Nickel Complexes Having Primary
 and Secondary Silyl Ligands
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2072
_journal_paper_doi               10.1021/om801187b
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         '2(C38 H51 Ni N P2 Si), C5 H12'
_chemical_formula_sum            'C40.5 H57 N Ni P2 Si'
_chemical_formula_weight         706.61
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 110.577(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.9191(13)
_cell_length_b                   10.3235(5)
_cell_length_c                   31.4006(16)
_cell_measurement_reflns_used    5296
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.35
_cell_volume                     7562.5(7)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2003)'
_computing_publication_material  'SHELXTL (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(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 90 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  0.0811
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            50579
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.9371
_exptl_absorpt_correction_T_min  0.8796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1997'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7751
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0718P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                5952
_reflns_number_total             7751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801187b_si_002.cif
_cod_data_source_block           07103
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C40.50 H57 N Ni P2 Si'
_cod_database_code               4068976