Steering S-H and N-H Bond Activation by a Stable N-Heterocyclic Silylene: Different Addition of H2S, NH3, and Organoamines on a Silicon(II) Ligand versus Its Si(II)→Ni(CO)3Complex
Antje Meltzer; Shigeyoshi Inoue; Carsten Präsang; Matthias Driess; Journal of the American Chemical Society 132 (2010) 3038–3046; doi:10.1021/ja910305p

data_4102022
_publ_section_title
;
 Steering S-H and N-H Bond Activation by a Stable N-Heterocyclic Silylene:
 Different Addition of H2S, NH3, and Organoamines on a Silicon(II) Ligand
 versus Its Si(II)\\rightarrowNi(CO)3Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3038
_journal_page_last               3046
_journal_paper_doi               10.1021/ja910305p
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C35 H46 N2 Ni Si'
_chemical_formula_sum            'C35 H46 N2 Ni Si'
_chemical_formula_weight         581.54
_chemical_name_common            LSi=Ni-(h6-C6H6)
_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
;
'Fri Oct 09 07:26:53 2009'
;
_audit_creation_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.494(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9717(2)
_cell_length_b                   16.5067(4)
_cell_length_c                   22.7886(7)
_cell_measurement_reflns_used    13889
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4468
_cell_measurement_theta_min      2.9830
_cell_volume                     3318.39(15)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26111
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.9383
_exptl_absorpt_correction_T_min  0.9095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5824
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0503P)^2^+0.6002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                4773
_reflns_number_total             5824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910305p_si_003.cif
_cod_data_source_block           m40
_cod_database_code               4102022