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_7035528
_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         'C9 H8 F15 N Si'
_chemical_formula_sum            'C9 H8 F15 N Si'
_chemical_formula_weight         443.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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_date             2014-03-07
_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                90.00
_cell_angle_beta                 92.425(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6077(3)
_cell_length_b                   15.7881(7)
_cell_length_c                   12.7448(6)
_cell_measurement_reflns_used    5970
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      27.7340
_cell_measurement_theta_min      2.9580
_cell_volume                     1529.42(12)
_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
;
SHELXH, 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 16.1901
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.8567
_diffrn_measurement_details
;
  1 omega  -35.00   52.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7120   57.0000 -180.0000 87

  2 omega  -80.00  -14.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7120  139.0000  -81.4378 66

  3 omega  -59.00  -34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7120  178.0000 -120.0000 25

  4 omega    4.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7120   57.0000  -30.0000 73

  5 omega  -52.00   27.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7120  -57.0000   60.0000 79

  6 omega  -20.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7120  -99.0000  -90.0000 77

  7 omega   28.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7120 -115.0000  115.0000 38

  8 omega    4.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7120   38.0000 -180.0000 83

  9 omega    4.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7120   57.0000 -120.0000 67

 10 omega   -8.00   10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7120   77.0000   60.0000 18
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0266832000
_diffrn_orient_matrix_UB_12      0.0417726000
_diffrn_orient_matrix_UB_13      -0.0123127000
_diffrn_orient_matrix_UB_21      0.0345565000
_diffrn_orient_matrix_UB_22      -0.0148903000
_diffrn_orient_matrix_UB_23      -0.0474183000
_diffrn_orient_matrix_UB_31      -0.0824100000
_diffrn_orient_matrix_UB_32      0.0072560000
_diffrn_orient_matrix_UB_33      -0.0265574000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16214
_diffrn_reflns_theta_full        24.9737
_diffrn_reflns_theta_max         28.9790
_diffrn_reflns_theta_min         2.58
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  1.652
_exptl_absorpt_correction_T_min  0.982
_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    1.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_crystal_preparation
'in situ grown at 155K and cooled down to 100K with 20 K/h.'
_exptl_crystal_size_max          0.3096
_exptl_crystal_size_mid          0.1906
_exptl_crystal_size_min          0.1808
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         2685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+1.7687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                2142
_reflns_number_total             2685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02010g2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7035526--7035529.cif.'
_cod_original_cell_volume        1529.41(12)
_cod_database_code               7035528
_chemical_oxdiff_formula         'C9 H8 F15 N Si'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97