Stable Silaimines with Three- and Four-Coordinate Silicon Atoms
Prinson P. Samuel; Ramachandran Azhakar; Rajendra S. Ghadwal; Sakya S. Sen; Herbert W. Roesky; Markus Granitzka; Julia Matussek; Regine Herbst-Irmer; Dietmar Stalke; Inorganic Chemistry 51 (2012) 11049–11054; doi:10.1021/ic301543y

data_4330703
_publ_section_title
;
 Stable Silaimines with Three- and Four-Coordinate Silicon Atoms
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11049
_journal_page_last               11054
_journal_paper_doi               10.1021/ic301543y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C65 H89 N3 Si'
_chemical_formula_sum            'C65 H89 N3 Si'
_chemical_formula_weight         940.48
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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                 93.35(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.144(2)
_cell_length_b                   12.315(2)
_cell_length_c                   22.761(3)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.678
_cell_measurement_theta_min      2.161
_cell_volume                     5636.7(13)
_computing_cell_refinement       'SAINT V7.68a'
_computing_data_collection       'APEX2 v2011.4-1'
_computing_data_reduction        'SAINT V7.68a'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart Apex Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            101565
_diffrn_reflns_theta_full        25.71
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         1.01
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.9702
_exptl_absorpt_correction_T_min  0.9139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2'
_exptl_crystal_colour            colorlesss
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         10683
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0371P)^2^+3.5779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                8776
_reflns_number_total             10683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301543y_si_001_1.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4330703