Pentacoordinate silicon(IV): cationic, anionic and neutral complexes derived from the reaction of NHC>SiCl4 with highly Lewis acidic (C2F5)2SiH2
T. Bottcher; S. Steinhauer; B. Neumann; H-G. Stammler; G.-V. Roschenthaler; B. Hoge; Chem.Commun. 50 (2014) 6204–; doi:10.1039/C4CC02583K

data_7113947
_publ_section_title
;
 Pentacoordinate silicon(IV): cationic, anionic and neutral complexes
 derived from the reaction of NHC>SiCl4 with highly Lewis acidic
 (C2F5)2SiH2
;
_journal_name_full               Chem.Commun.
_journal_page_first              6204
_journal_paper_doi               10.1039/C4CC02583K
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C5 H10.90458 Cl3.09542 N2 Si'
_chemical_formula_sum            'C5 H10.90458 Cl3.09543 N2 Si'
_chemical_formula_weight         236.88
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-10-07
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.05642(14)
_cell_length_b                   10.62115(11)
_cell_length_c                   14.80917(14)
_cell_measurement_reflns_used    80661
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      40.8150
_cell_measurement_theta_min      3.8120
_cell_volume                     2053.65(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 5.3114
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9880
_diffrn_measurement_details
;
  1 omega  -40.00   -5.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012  -83.0000 -100.2655 35

  2 omega  -45.00   -6.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012  -82.0000  160.7464 39

  3 omega  -58.00   20.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012   38.0000  -90.0000 78

  4 omega  -46.00   -6.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012  -81.0000   67.5613 40

  5 omega  -45.00   -6.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012  -81.0000  -27.5407 39

  6 omega   18.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262   38.0000  -60.0000 91

  7 omega   -9.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262  -99.0000  -30.0000 86

  8 omega   19.00  108.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262   38.0000 -150.0000 89

  9 omega    0.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262 -122.0000 -160.2961 90

 10 omega   42.00   98.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262  178.0000  150.0000 56

 11 omega   17.00  106.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262   38.0000   30.0000 89

 12 omega   17.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262   38.0000  120.0000 92

 13 omega  -16.00   30.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262  -99.0000   30.0000 46

 14 omega   11.00   96.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262 -132.0000  160.8764 85

 15 omega -121.00  -57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012 -178.0000   60.0000 64

 16 omega -121.00  -57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012 -178.0000 -180.0000 64

 17 omega  -40.00   -5.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012  -83.0000   90.5115 35

 18 omega -122.00  -55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012  178.0000  -60.0000 67

 19 omega   17.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262   38.0000 -120.0000 92

 20 omega   35.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262  178.0000    0.0000 86

 21 omega   13.00  106.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262   57.0000  -60.0000 93

 22 omega  -30.00   63.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262  -57.0000  -30.0000 93

 23 omega   13.00  106.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262   57.0000   30.0000 93

 24 omega  -39.00   71.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262  -19.0000   60.0000 110

 25 omega   13.00  106.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262   57.0000  120.0000 93

 26 omega  -58.00   34.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012   38.0000   60.0000 92

 27 omega -108.00  -17.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012  -38.0000  150.0000 91

 28 omega  -67.00   34.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012   77.0000  150.0000 101

 29 omega  -45.00   -6.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012  -82.0000  160.7464 39

 30 omega  -46.00   -6.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012  -81.0000  -27.5407 40

 31 omega -109.00   -7.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3012  -77.0000   60.0000 102

 32 omega  -20.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262  -99.0000   30.0000 97

 33 omega  -20.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262  -99.0000 -120.0000 97

 34 omega  -33.00   59.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262  -38.0000 -150.0000 92

 35 omega    6.00   96.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       37.9262 -132.0000  160.8764 90
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0048343000
_diffrn_orient_matrix_UB_12      -0.0641819000
_diffrn_orient_matrix_UB_13      0.0125103000
_diffrn_orient_matrix_UB_21      0.0409467000
_diffrn_orient_matrix_UB_22      0.0157662000
_diffrn_orient_matrix_UB_23      0.0293767000
_diffrn_orient_matrix_UB_31      -0.0353630000
_diffrn_orient_matrix_UB_32      0.0095270000
_diffrn_orient_matrix_UB_33      0.0357172000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0070
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            136389
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         2.829
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_T_max  1.374
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       irregular
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.2623
_exptl_crystal_size_mid          0.2419
_exptl_crystal_size_min          0.1837
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         3005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0267P)^2^+1.9222P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2925
_reflns_number_total             3005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02583k2.cif
_cod_data_source_block           compound6
_cod_database_code               7113947
_chemical_oxdiff_formula         'C5 H10 Cl3 N2 Si'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     39.98
_shelx_res_checksum              66222
_shelxl_version_number           2013-2