Diketiminate Silicon(II) and Related NHSi Ligands Generated in the Coordination Sphere of Nickel(0)
Antje Meltzer; Carsten Präsang; Matthias Driess; Journal of the American Chemical Society 131 (2009) 7232–7233; doi:10.1021/ja9026727

data_4104459
_publ_contact_author_address
;Technische Universit\"at Berlin,
Institute of Chemistry
Strasse des 17. Juni 136, D-10623 Berlin, Germany
;
_publ_contact_author_email       matthias.driess@tu-berlin.de
_publ_contact_author_fax         +49(0)30-314-29732
_publ_contact_author_name        'Matthias Driess'
_publ_contact_author_phone       +49(0)30-314-29731
_publ_section_title
;
 Diketiminate Silicon(II) and Related NHSi Ligands Generated in the
 Coordination Sphere of Nickel(0)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7232
_journal_page_last               7233
_journal_paper_doi               10.1021/ja9026727
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C107 H88 B2 F30 N4 Ni2 O6 Si2'
_chemical_formula_sum            'C107 H88 B2 F30 N4 Ni2 O6 Si2'
_chemical_formula_weight         2291.03
_chemical_name_common            '(C6F5)3B-LSi=Ni(CO)3 * 1/2 toluene'
_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
;
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                64.292(3)
_cell_angle_beta                 71.710(3)
_cell_angle_gamma                87.140(2)
_cell_formula_units_Z            2
_cell_length_a                   14.6855(3)
_cell_length_b                   20.2466(7)
_cell_length_c                   20.5691(7)
_cell_measurement_reflns_used    12909
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3719
_cell_measurement_theta_min      2.9269
_cell_volume                     5205.4(3)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0883
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42859
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.9430
_exptl_absorpt_correction_T_min  0.9075
_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            yellow
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1396
_refine_ls_number_reflns         18200
_refine_ls_number_restraints     882
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0532P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                11431
_reflns_number_total             18200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9026727_si_004.cif
_cod_data_source_block           m27
_cod_database_code               4104459