Donor-Stabilized Silyl Cations. 11. Bis-Zwitterionic Penta- and Hexacoordinate Silicon Dichelate Complexes Derived from (ClCH2)2SiCl2through Double Internal Displacement of Chloride1
Gostevskii, Boris; Zamstein, Noa; Korlyukov, Alexander A.; Baukov, Yuri I.; Botoshansky, Mark; Kaftory, Menahem; Kocher, Nikolaus; Stalke, Dietmar; Kalikhman, Inna; Kost, Daniel; Organometallics 25 (2006) 5416–; doi:10.1021/om060629w

data_4074422
_publ_contact_author             'Prof. D. Kost & Prof. Dr. D. Stalke'
_publ_section_title
;
 Donor-Stabilized Silyl Cations. 11. Bis-Zwitterionic Penta- and
 Hexacoordinate Silicon Dichelate Complexes Derived from
 (ClCH2)2SiCl2through Double Internal Displacement of Chloride1
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5416
_journal_paper_doi               10.1021/om060629w
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C24 H38 Cl2 F12 N10 O5 Si2'
_chemical_formula_weight         901.72
_chemical_name_common            11a
_chemical_name_systematic
; 
 Di(Bis-(N,N-dimethyl-N-trifluoroacetimidato-ammoniomethyl-C-O)disiloxane-dication dichloride 
;
_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                 95.2290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4375(6)
_cell_length_b                   18.3791(10)
_cell_length_c                   20.7842(11)
_cell_measurement_reflns_used    7882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.499
_cell_measurement_theta_min      2.251
_cell_volume                     3970.5(4)
_computing_cell_refinement       'SAINT-NT V5/6.0'
_computing_data_collection       'SMART-NT V5.624'
_computing_data_reduction        'SAINT-NT V5/6.0'
_computing_molecular_graphics    'XP in SHELXL-97'
_computing_publication_material  'XP in SHELXL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex on D8-Goniometer'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0124
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            39662
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.873248
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS2.0 (Sheldrick 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+2.3877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                6809
_reflns_number_total             7388
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            om060629wsi20060713_094327.cif
_cod_data_source_block           11a
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C12 H19 Cl F6 N5 O2.50 Si'
_cod_database_code               4074422