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_7113946
_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         'C4 Cl3 F10 Si, C10 H21 Cl2 N4 Si'
_chemical_formula_sum            'C14 H21 Cl5 F10 N4 Si2'
_chemical_formula_weight         668.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-03-13
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                89.833(2)
_cell_angle_beta                 81.713(2)
_cell_angle_gamma                79.902(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1924(2)
_cell_length_b                   12.5273(3)
_cell_length_c                   13.0812(3)
_cell_measurement_reflns_used    18021
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      76.2520
_cell_measurement_theta_min      3.4010
_cell_volume                     1307.56(5)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
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    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector_area_resol_mean 5.3114
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.9863
_diffrn_measurement_details
;
  1 omega  -43.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -61.0000    0.0000 30

  2 omega  -48.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   30.0000  120.0000 83

  3 omega -105.00  -59.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -61.0000    0.0000 46

  4 omega -111.00  -67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -30.0000   90.0000 44

  5 omega  -60.00  -18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -30.0000   90.0000 42

  6 omega -121.00  -44.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000 -178.0000   90.0000 77

  7 omega   58.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000   30.0000 50

  8 omega   72.00   99.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000 -150.0000 27

  9 omega   13.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  150.0000 56

 10 omega   84.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  150.0000 29

 11 omega   13.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000   60.0000 100

 12 omega   30.00   56.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000  -30.0000 26

 13 omega   30.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000 -150.0000 25

 14 omega   13.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -30.0000 59

 15 omega   49.00   95.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000  150.0000 46

 16 omega   70.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000  -30.0000 44

 17 omega   60.00  125.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000  150.0000 65

 18 omega   13.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -120.0000 60

 19 omega   85.00  156.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 71

 20 omega   85.00  111.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 26

 21 omega   81.00  127.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 46

 22 omega   85.00  160.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 75

 23 omega   85.00  167.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 82

 24 omega   85.00  171.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 86

 25 omega   85.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 93

 26 omega   44.00  121.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 77

 27 omega   85.00  173.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 88

 28 omega   89.00  177.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   60.0000 88

 29 omega   85.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 29

 30 omega   85.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 29

 31 omega   32.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 77

 32 omega   81.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 27

 33 omega   31.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 57

 34 omega  119.00  173.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 54

 35 omega   50.00  137.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  120.0000 87

 36 omega   41.00   94.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -30.0000 53

 37 omega  128.00  167.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 39

 38 omega   81.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 33

 39 omega   81.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 26

 40 omega   81.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 26

 41 omega   81.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 32

 42 omega   81.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 26

 43 omega   81.00  175.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 94

 44 omega   61.00  121.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  120.0000 60

 45 omega   81.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 26

 46 omega   32.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 40

 47 omega   85.00  111.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 26

 48 omega   81.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 26

 49 omega   85.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 27

 50 omega   81.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 26

 51 omega   54.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 48

 52 omega   83.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   71.0000  138.7910 95

 53 omega   85.00  136.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -133.9883 51
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1322727000
_diffrn_orient_matrix_UB_12      -0.0035325000
_diffrn_orient_matrix_UB_13      -0.0719572000
_diffrn_orient_matrix_UB_21      0.0499428000
_diffrn_orient_matrix_UB_22      -0.1243855000
_diffrn_orient_matrix_UB_23      -0.0092468000
_diffrn_orient_matrix_UB_31      -0.1314779000
_diffrn_orient_matrix_UB_32      -0.0112630000
_diffrn_orient_matrix_UB_33      0.0943817000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22010
_diffrn_reflns_theta_full        71.98
_diffrn_reflns_theta_max         71.98
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.743
_exptl_absorpt_correction_T_max  1.022
_exptl_absorpt_correction_T_min  0.367
_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    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             672
_exptl_crystal_recrystallization_method
;
Disorder of C(2), F(3), F(4), and F(5) on two positions (90:10).
Disorder of F(8), F(9), and F(10) on two positions (90:10). Hydogens were refined isotropically.
;
_exptl_crystal_size_max          0.3834
_exptl_crystal_size_mid          0.0992
_exptl_crystal_size_min          0.0876
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         5116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0290P)^2^+0.7984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                4967
_reflns_number_total             5116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02583k2.cif
_cod_data_source_block           compound5
_cod_original_cell_volume        1307.57(6)
_cod_database_code               7113946
_chemical_oxdiff_formula         'C5 H10 B Cl7 N2 Si'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98