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_4115556
_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            'C24.5 H34.5 Cl9.5 N4 O3 Si2'
_chemical_formula_weight         826.02
_chemical_name_common            'Chloro-bridged disiloxane (15) '
_chemical_name_systematic
; 
 bis-[(1-((1,1-dimethyl-2-benzoylhydrazonium)methyl-C,O)methyl]disiloxane 
dichloride 
;
_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                 95.20(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.311(2)
_cell_length_b                   17.410(4)
_cell_length_c                   19.369(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.22
_cell_measurement_theta_min      3.83
_cell_volume                     3798.5(14)
_computing_cell_refinement       'STOE Cell'
_computing_data_collection       'STOE Expose'
_computing_data_reduction        'STOE Integrate'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  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 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'Phi 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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0728
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20472
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.7966
_exptl_absorpt_correction_T_min  0.6473
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         4939
_refine_ls_number_restraints     327
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                3031
_reflns_number_total             5144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja004118r_2.cif
_cod_data_source_block           15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3798.7(13)
_cod_original_formula_sum        'C24.50 H34.50 Cl9.50 N4 O3 Si2'
_cod_database_code               4115556