Tautomeric Equilibrium between Penta- and Hexacoordinate Silicon Chelates. A Chloride Bridge between Two Pentacoordinate Silicons
Inna Kalikhman; Olga Girshberg; Lutz Lameyer; Dietmar Stalke; Daniel Kost; Journal of the American Chemical Society 123 (2001) 4709–4716; doi:10.1021/ja004118r

data_4115557
_publ_section_title
;
 Tautomeric Equilibrium between Penta- and Hexacoordinate Silicon
 Chelates. A Chloride Bridge between Two Pentacoordinate Silicons
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4709
_journal_page_last               4716
_journal_paper_doi               10.1021/ja004118r
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C9 H20 Cl4 N4 O2 Si'
_chemical_formula_weight         386.18
_chemical_name_common            11b
_chemical_name_systematic
; 
 (N-(dimethylamino)formimidato-N,O)
(1-((1,1-dimethyl-2-formylhydrazonium)methyl-C,O)methylsilicon(IV) chloride 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.496(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.1313(11)
_cell_length_b                   21.369(4)
_cell_length_c                   6.7900(12)
_cell_measurement_temperature    173(2)
_cell_volume                     879.9(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12228
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.4
_refine_diff_density_max         2.527
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4113
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1805P)^2^+0.6268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2323
_refine_ls_wR_factor_ref         0.2364
_reflns_number_gt                3756
_reflns_number_total             4113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja004118r_3.cif
_cod_data_source_block           11b
_cod_database_code               4115557