Hypercoordinate Organosilicon Complexes of an ONN′O′ Chelating Ligand: Regio- and Diastereoselectivity of Rearrangement Reactions in Si−Salphen Systems
Lippe, Katrin; Gerlach, Daniela; Kroke, Edwin; Wagler, Jörg; Organometallics 28 (2009) 621–; doi:10.1021/om801049q

data_4068709
_publ_section_title
;
 Hypercoordinate Organosilicon Complexes of an ONN&#x2032;O&#x2032;
 Chelating Ligand: Regio- and Diastereoselectivity of Rearrangement
 Reactions in Si&#x2212;Salphen Systems
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              621
_journal_paper_doi               10.1021/om801049q
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C39 H30 N2 O3 Si, C H Cl3'
_chemical_formula_sum            'C40 H31 Cl3 N2 O3 Si'
_chemical_formula_weight         722.11
_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
_cell_angle_alpha                119.1980(10)
_cell_angle_beta                 98.988(2)
_cell_angle_gamma                98.715(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9840(6)
_cell_length_b                   13.4905(3)
_cell_length_c                   13.6978(3)
_cell_measurement_reflns_used    9661
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      33.46
_cell_measurement_theta_min      2.27
_cell_volume                     1687.93(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP32 (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25162
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.351
_exptl_absorpt_correction_T_max  0.9332
_exptl_absorpt_correction_T_min  0.8273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.334
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         9728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.334
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0632P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1308
_reflns_number_gt                7728
_reflns_number_total             9728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801049q_si_001.cif
_cod_data_source_block           compound_5a
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068709