Tridentate Lewis-acids based on triphenylsilane.
Tomaschautzky, Janek; Neumann, Beate; Stammler, Hans-Georg; Mix, Andreas; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1645–1659; doi:10.1039/c6dt04293g

data_7041638
_publ_section_title
;
 Tridentate Lewis-acids based on triphenylsilane.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1645
_journal_page_last               1659
_journal_paper_doi               10.1039/c6dt04293g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C18 H12 F1 I3 Si1, 0.5 (C5 H12)squeezed'
_chemical_formula_sum            'C20.5 H18 F I3 Si'
_chemical_formula_weight         692.14
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.12 svn.r2899 for OlexSys, GUI svn.r4796)
;
_audit_update_record
;
2016-10-28 deposited with the CCDC.
2017-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.5289(4)
_cell_length_b                   14.5289(4)
_cell_length_c                   5.78666(15)
_cell_measurement_reflns_used    8387
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.1190
_cell_measurement_theta_min      3.4570
_cell_volume                     1057.85(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9967
_diffrn_measurement_details
;
  1 omega  -41.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000 -120.0000 28

  2 omega -109.00  -57.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000 -158.0000 -103.0000 52

  3 omega -102.00  -75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000 -120.0000 27

  4 omega  -43.00   -6.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000    0.0000 37

  5 omega   69.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000  -90.0000 45

  6 omega   18.00   61.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000  150.0000 43

  7 omega  -32.00   57.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488  -19.0000  150.0000 89

  8 omega   16.00   56.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000  -30.0000 40

  9 omega   16.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000   90.0000 98

 10 omega   13.00   59.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000  -90.0000 46

 11 omega   65.00  125.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488  178.0000   30.0000 60

 12 omega   13.00   65.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000   30.0000 52

 13 omega   58.00  101.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488  178.0000  -90.0000 43

 14 omega   26.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   38.0000   30.0000 50

 15 omega    1.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488  -99.0000   90.0000 81

 16 omega   15.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000 -150.0000 97

 17 omega   68.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000  150.0000 35

 18 omega   81.00  124.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 43

 19 omega   48.00  141.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -120.0000 93

 20 omega   31.00  105.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 74

 21 omega   98.00  136.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  -30.0000 38

 22 omega   85.00  112.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 27

 23 omega   85.00  178.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 93

 24 omega   82.00  109.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 27

 25 omega   81.00  108.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 27

 26 omega   85.00  112.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 27

 27 omega  133.00  161.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 28

 28 omega   85.00  125.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 40

 29 omega   86.00  111.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 25

 30 omega   85.00  121.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 36

 31 omega   82.00  107.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   76.0000   50.6959 25

 32 omega   32.00  109.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 77

 33 omega   43.00   68.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 25

 34 omega   81.00  107.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 26

 35 omega   82.00  178.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 96

 36 omega   85.00  159.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 74

 37 omega   81.00  108.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 27

 38 omega   86.00  162.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 76

 39 omega   85.00  178.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 93

 40 omega   41.00   97.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 56

 41 omega   82.00  173.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 91

 42 omega   82.00  122.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 40

 43 omega   85.00  178.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 93

 44 omega  129.00  170.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 41

 45 omega  126.00  177.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 51

 46 omega   85.00  113.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 28

 47 omega   86.00  111.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 25

 48 omega   81.00  107.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 26

 49 omega   81.00  178.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 97

 50 omega   81.00  107.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 26

 51 omega   83.00  121.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   67.0000 -108.2479 38

 52 omega  119.00  146.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   76.0000  124.4213 27

 53 omega   47.00  109.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 62

 54 omega   82.00  109.00   1.0000    3.2000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   76.0000  124.4213 27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0304493000
_diffrn_orient_matrix_UB_12      0.0059868000
_diffrn_orient_matrix_UB_13      -0.2523455000
_diffrn_orient_matrix_UB_21      -0.0757184000
_diffrn_orient_matrix_UB_22      -0.1211454000
_diffrn_orient_matrix_UB_23      -0.0011844000
_diffrn_orient_matrix_UB_31      -0.0912631000
_diffrn_orient_matrix_UB_32      0.0164325000
_diffrn_orient_matrix_UB_33      0.0850580000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            17665
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.46
_diffrn_reflns_theta_min         3.51
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    35.435
_exptl_absorpt_correction_T_max  0.294
_exptl_absorpt_correction_T_min  0.019
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.173
_exptl_crystal_description       needle
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.1942
_exptl_crystal_size_mid          0.0384
_exptl_crystal_size_min          0.0329
_refine_diff_density_max         0.452
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack x determined using 652 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1379
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0544P)^2^+0.9088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.978
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1350
_reflns_number_total             1379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma06_1
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_original_cell_volume        1057.85(6)
_cod_original_formula_sum        'C20.50 H18 F I3 Si'
_cod_database_code               7041638
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C18 H12 I3 Si F'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed U13: Si1(0) F1(0)
 Fixed U23: Si1(0) F1(0)
 Fixed Uiso: H3(0.041) H4(0.052) H5(0.048) H6(0.041)
 Fixed X: Si1(0.3333) F1(0.3333) H3(0.1203) H4(0.2213) H5(0.3752) H6(0.4193)
 Fixed Y: Si1(0.6667) F1(0.6667) H3(0.2773) H4(0.2724) H5(0.4267) H6(0.5859)
 Fixed Z: H3(0.5102) H4(0.8083) H5(0.9243) H6(0.7453)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'