Synthesis, structure and reactivity of a donor-stabilised silylene with a bulky bidentate benzamidinato ligand.
Tacke, Reinhold; Kobelt, Claudia; Baus, Johannes A.; Bertermann, Rüdiger; Burschka, Christian; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14959–14974; doi:10.1039/c5dt01581b

data_7036018
_publ_section_title
;
 Synthesis, structure and reactivity of a donor-stabilised silylene with a
 bulky bidentate benzamidinato ligand.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14959
_journal_page_last               14974
_journal_paper_doi               10.1039/c5dt01581b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C33 H45 N3 Si'
_chemical_formula_sum            'C33 H45 N3 Si'
_chemical_formula_weight         511.81
_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           SHELXL-97
_audit_update_record
;
2015-04-23 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                99.41(3)
_cell_angle_beta                 98.90(3)
_cell_angle_gamma                97.53(3)
_cell_formula_units_Z            2
_cell_length_a                   9.049(5)
_cell_length_b                   9.540(3)
_cell_length_c                   18.295(8)
_cell_measurement_reflns_used    6212
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.83
_cell_measurement_theta_min      2.19
_cell_volume                     1519.4(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP/POV-Ray
_computing_publication_material  Bruker-SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17741
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.9792
_exptl_absorpt_correction_T_min  0.9413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0423P)^2^+0.6708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                4879
_reflns_number_total             5986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01581b1.cif
_cod_data_source_block           kob40c
_cod_depositor_comments
'Adding full bibliography for 7036018--7036028.cif.'
_cod_original_cell_volume        1519.5(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7036018