Pentafluoroethyl-substituted α-silanes: model compounds for new insights.
Waerder, Benedikt; Steinhauer, Simon; Bader, Julia; Neumann, Beate; Stammler, Hans-Georg; Vishnevskiy, Yury V.; Hoge, Berthold; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13347–13358; doi:10.1039/c5dt02010g

data_7035529
_publ_section_title
;
 Pentafluoroethyl-substituted \a-silanes: model compounds for new
 insights.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13347
_journal_page_last               13358
_journal_paper_doi               10.1039/c5dt02010g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C8 H6 F15 N O Si'
_chemical_formula_sum            'C8 H6 F15 N O Si'
_chemical_formula_weight         445.23
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-09
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2015-05-20 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                105.422(7)
_cell_angle_beta                 91.660(5)
_cell_angle_gamma                104.381(6)
_cell_formula_units_Z            4
_cell_length_a                   8.0664(3)
_cell_length_b                   13.2774(13)
_cell_length_c                   14.9990(10)
_cell_measurement_reflns_used    35277
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      31.5800
_cell_measurement_theta_min      1.6540
_cell_volume                     1492.3(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9995
_diffrn_measurement_details
;
  1 omega  -13.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489   19.0000  -30.0000 110

  2 omega   -4.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489   77.0000 -120.0000 98

  3 omega    6.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489   57.0000  120.0000 87

  4 omega  -20.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489  -99.0000  150.0000 85

  5 omega   -4.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489   77.0000  -30.0000 98

  6 omega   35.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489  178.0000   30.0000 64

  7 omega  -44.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489  -77.0000   30.0000 98

  8 omega  -20.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489  -99.0000  -90.0000 85

  9 omega   -4.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489   77.0000  150.0000 98

 10 omega    6.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489   57.0000   90.0000 87

 11 omega  -47.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489  -19.0000  150.0000 110

 12 omega  -84.00   -8.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  134.0000 -129.7919 76

 13 omega  -93.00    5.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -77.0000    0.0000 98

 14 omega  -95.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -180.0000 143

 15 omega  -92.00   -5.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -57.0000 -180.0000 87

 16 omega    0.00   78.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489 -123.0000 -135.0000 78

 17 omega   35.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489  178.0000 -180.0000 64

 18 omega   14.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489 -150.0000   62.0000 82

 19 omega    3.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489   38.0000   60.0000 93

 20 omega  -20.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9489  -99.0000  -30.0000 85

 21 omega  -95.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -120.0000 143

 22 omega  -95.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  -90.0000 143

 23 omega  -95.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  -60.0000 141

 24 omega  -95.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -150.0000 143
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0345482000
_diffrn_orient_matrix_UB_12      0.0528422000
_diffrn_orient_matrix_UB_13      -0.0044551000
_diffrn_orient_matrix_UB_21      -0.0044123000
_diffrn_orient_matrix_UB_22      -0.0218086000
_diffrn_orient_matrix_UB_23      -0.0489011000
_diffrn_orient_matrix_UB_31      -0.0843911000
_diffrn_orient_matrix_UB_32      0.0062402000
_diffrn_orient_matrix_UB_33      -0.0047139000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            87610
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.031
_diffrn_reflns_theta_min         1.847
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_description       cylindrically
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.4893
_exptl_crystal_size_mid          0.2229
_exptl_crystal_size_min          0.2032
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         8724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0354P)^2^+0.8112P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7516
_reflns_number_total             8724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02010g2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7035526--7035529.cif.'
_cod_original_cell_volume        1492.26(19)
_cod_database_code               7035529
_chemical_oxdiff_formula         'C8 H6 F15 N O Si'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_shelx_res_checksum              10133
_shelxl_version_number           2013-2