Equilibrium between neutral hexacoordinate silicon complexes and ionic pentacoordinate siliconium salts through fast dissociation–recombination of the Si–Cl bond
Kingston, Vijeyakumar; Gostevskii, Boris; Kalikhman, Inna; Kost, Daniel; Chemical Communications  (2001) 1272–; doi:10.1039/b102427m

data_7115000
_publ_section_title
;
 Equilibrium between neutral hexacoordinate silicon complexes and ionic
 pentacoordinate siliconium salts through fast dissociation--recombination
 of the Si--Cl bond
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1272
_journal_paper_doi               10.1039/b102427m
_journal_year                    2001
_chemical_formula_sum            'C20 H22 F6 N4 O8 S2 Si'
_chemical_formula_weight         652.63
_chemical_melting_point          '193-5 &#x00A1;C '
_chemical_name_common            7
_chemical_name_systematic
; 
Bis(N,N-dimethylbenzhydrazido-N,O)-bis(trifluoromethylsulfonyl)silicon 
;
_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                 102.427(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.466(5)
_cell_length_b                   8.193(3)
_cell_length_c                   20.861(7)
_cell_measurement_temperature    173(2)
_cell_volume                     2748.3(16)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26602
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         3920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0462P)^2^+6.3094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                3163
_reflns_number_total             3920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102427m.txt
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2748.3(15)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7115000