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_7113948
_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 H12 Cl2 N2 Si'
_chemical_formula_sum            'C5 H12 Cl2 N2 Si'
_chemical_formula_weight         199.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-06-06
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.020(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9722(3)
_cell_length_b                   12.2770(3)
_cell_length_c                   7.76332(14)
_cell_measurement_reflns_used    19302
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      32.1400
_cell_measurement_theta_min      3.8760
_cell_volume                     950.45(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
;
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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector_area_resol_mean 5.3114
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9704
_diffrn_measurement_details
;
  1 omega  -75.00  -50.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -      -17.0167  131.0000  114.6288 25

  2 omega  -72.00  -47.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -      -17.0167  126.0000  -78.8396 25

  3 omega  -90.00  -63.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -      -17.0167  153.0000  177.5752 27

  4 omega   -9.00   88.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417   77.0000  -90.0000 97

  5 omega   -5.00   84.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417   77.0000  120.0000 89

  6 omega   11.00   79.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417   57.0000   30.0000 68

  7 omega    7.00   89.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417   38.0000 -120.0000 82

  8 omega  -51.00   32.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417  -38.0000 -150.0000 83

  9 omega  -53.00   37.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417  -38.0000  120.0000 90

 10 omega  -38.00   41.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417  -57.0000  -60.0000 79

 11 omega   18.00   92.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417 -155.0000  124.6126 74

 12 omega -101.00  -55.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -      -17.0167  178.0000   60.0000 46

 13 omega  -42.00   51.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -      -17.0167   57.0000  150.0000 93

 14 omega  -90.00  -38.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -      -17.0167  153.0000  -42.3990 52

 15 omega  -53.00   38.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417  -38.0000  -30.0000 91

 16 omega   -8.00   86.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417   57.0000  150.0000 94

 17 omega   -3.00   89.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417   38.0000  -90.0000 92

 18 omega   -3.00   89.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417   38.0000   60.0000 92

 19 omega   35.00  101.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417  178.0000    0.0000 66

 20 omega  -20.00   56.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417  -99.0000  120.0000 76

 21 omega  -76.00  -29.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -      -17.0167  133.0000   65.8364 47

 22 omega -101.00  -55.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -      -17.0167  178.0000  120.0000 46

 23 omega  -47.00   54.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -      -17.0167   77.0000 -120.0000 101

 24 omega  -85.00    8.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -      -17.0167  -57.0000 -120.0000 93

 25 omega  -84.00  -34.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -      -17.0167  146.0000   22.3998 50

 26 omega  -86.00  -35.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -      -17.0167  148.0000  143.7601 51

 27 omega   35.00  101.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417  178.0000  -90.0000 66

 28 omega   18.00   92.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417 -155.0000  124.6126 74

 29 omega   11.00   81.00   1.0000   13.3400
omega____ theta____ kappa____ phi______ frames
    -       17.6417 -140.0000 -165.9973 70
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0005906000
_diffrn_orient_matrix_UB_12      0.0390545000
_diffrn_orient_matrix_UB_13      -0.0673571000
_diffrn_orient_matrix_UB_21      -0.0709247000
_diffrn_orient_matrix_UB_22      -0.0036843000
_diffrn_orient_matrix_UB_23      -0.0043905000
_diffrn_orient_matrix_UB_31      -0.0056625000
_diffrn_orient_matrix_UB_32      0.0423487000
_diffrn_orient_matrix_UB_33      0.0616428000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            56379
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.997
_diffrn_reflns_theta_min         3.105
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  1.178
_exptl_absorpt_correction_T_min  0.878
_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    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.1623
_exptl_crystal_size_mid          0.1418
_exptl_crystal_size_min          0.1098
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2767
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+1.3632P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2649
_reflns_number_total             2767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02583k2.cif
_cod_data_source_block           compound7
_cod_database_code               7113948
_chemical_oxdiff_formula         'C5 H12 Cl2 N2 Si'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_shelx_res_checksum              93282
_shelxl_version_number           2013-2