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_4115555
_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            'C6 H11 Cl2 F3 N2 O Si'
_chemical_formula_weight         283.16
_chemical_name_common            9a
_chemical_name_systematic
; 
(1-((1,1-dimethyl-2-trifluoroacetyl)hydrazonim)methyl-C,O)
methyldichlorosilicon(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.68(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.487(2)
_cell_length_b                   7.1123(6)
_cell_length_c                   13.738(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1206.1(4)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        XCAD4b
_computing_molecular_graphics    'Bruker SHELXTL-Plus'
_computing_publication_material  'Bruker SHELXTL-Plus'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       2theta/omega
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2303
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.7361
_exptl_absorpt_correction_T_min  0.6955
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       prisms
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0039(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+0.9968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                1844
_reflns_number_total             2125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja004118r_1.cif
_cod_data_source_block           9a
_cod_original_cell_volume        1206.1(3)
_cod_database_code               4115555