Synthesis and Reactivity of Silyl Iron, Cobalt, and Nickel Complexes Bearing a [PSiP]-Pincer Ligand via Si‒H Bond Activation
Wu, Siquan; Li, Xiaoyan; Xiong, Zichang; Xu, Wengang; Lu, Yunqiang; Sun, Hongjian; Organometallics 32 (2013) 3227–; doi:10.1021/om400047j

data_4089406
_publ_section_title
;
 Synthesis and Reactivity of Silyl Iron, Cobalt, and Nickel Complexes
 Bearing a [PSiP]-Pincer Ligand via Si--H Bond Activation
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3227
_journal_paper_doi               10.1021/om400047j
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C40 H40 Cl Co P3 Si'
_chemical_formula_sum            'C40 H40 Cl Co P3 Si'
_chemical_formula_weight         736.10
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_H-M   'P 1 21/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                 97.750(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.199(3)
_cell_length_b                   9.7500(19)
_cell_length_c                   22.438(5)
_cell_measurement_reflns_used    18304
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      1.27
_cell_volume                     3511.5(12)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      ' 212 frames, detector distance = 120 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15416
_diffrn_reflns_theta_full        26.82
_diffrn_reflns_theta_max         26.82
_diffrn_reflns_theta_min         1.27
_diffrn_source_current           150
_diffrn_source_power             7.50
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         7349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0583
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1700
_reflns_number_gt                4994
_reflns_number_total             7349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400047j_si_002.cif
_cod_data_source_block           complex15
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4089406