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_7041632
_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
'0.975(C24 H30 Br3 F Si4), 0.025(C24 H30 Br4 Si4)'
_chemical_formula_sum            'C24 H30 Br3.03 F0.97 Si4'
_chemical_formula_weight         691.12
_chemical_name_systematic
;
 ?
;
_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     dual
_audit_creation_date             2015-01-14
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2016-10-28 deposited with the CCDC.
2017-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                98.4221(10)
_cell_angle_beta                 103.5283(11)
_cell_angle_gamma                104.8703(12)
_cell_formula_units_Z            2
_cell_length_a                   10.21572(13)
_cell_length_b                   11.13196(15)
_cell_length_c                   13.90239(16)
_cell_measurement_reflns_used    63018
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.3210
_cell_measurement_theta_min      3.2940
_cell_volume                     1449.33(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
SHELXD, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(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 0.9941
_diffrn_measurement_details
;
  1 omega -116.00   -5.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000  -30.0000 111

  2 omega  -50.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  150.0000 83

  3 omega -122.00  -35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000 -178.0000 -180.0000 87

  4 omega   18.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000 -180.0000 94

  5 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  150.0000 102

  6 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -30.0000 102

  7 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -60.0000 102

  8 omega   23.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000  120.0000 91

  9 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -150.0000 102

 10 omega   57.00  127.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000  120.0000 70

 11 omega   57.00  127.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000  -60.0000 70

 12 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000   60.0000 102

 13 omega   23.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000   30.0000 91

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

 15 omega   31.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 78

 16 omega   82.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   71.0000 -177.7710 96

 17 omega   40.00  141.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000   90.0000 101

 18 omega   89.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -120.0000 89

 19 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 97

 20 omega   85.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 93

 21 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 97

 22 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 97

 23 omega   82.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   74.0000  -94.8217 96

 24 omega   41.00  122.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  120.0000 81

 25 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 97

 26 omega   85.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 93

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

 28 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 97

 29 omega   85.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 93

 30 omega   41.00  122.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -30.0000 81

 31 omega   82.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   72.0000   87.9235 96

 32 omega   85.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 93

 33 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 97

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

 35 omega   85.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 93

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

 37 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 97

 38 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 97

 39 omega   36.00  143.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -84.0000 -127.0000 107

 40 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 97

 41 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 97

 42 omega   31.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 78

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

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

 45 omega   31.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 78

 46 omega   83.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   70.0000 -131.4605 95

 47 omega   84.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   66.0000  -49.2386 94

 48 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   48.8980 97

 49 omega   82.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   74.0000   22.5049 96

 50 omega  -50.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000    0.0000 83

 51 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000 -150.0000 171

 52 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000 -180.0000 171

 53 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000  -90.0000 171

 54 omega   23.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000   60.0000 91

 55 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000    0.0000 171

 56 omega   23.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000   90.0000 91

 57 omega   23.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000 -150.0000 91

 58 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000  -30.0000 171

 59 omega   23.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000 -120.0000 91

 60 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -120.0000 102

 61 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000 -120.0000 171

 62 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000  -60.0000 171

 63 omega   18.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  120.0000 94

 64 omega   18.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  -30.0000 94

 65 omega   91.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   36.0000 -147.2912 87

 66 omega   31.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  150.0000 78

 67 omega   41.00   99.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -180.0000 58

 68 omega   89.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   60.0000 89

 69 omega   89.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   30.0000 89

 70 omega   89.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000    0.0000 89

 71 omega   90.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  120.0000 88

 72 omega   89.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -90.0000 89

 73 omega   89.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -180.0000 89

 74 omega   26.00  174.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000    0.0000    0.0000 148

 75 omega   89.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  150.0000 89

 76 omega   26.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000    0.0000  -30.0000 152

 77 omega   41.00   99.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 58

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

 79 omega   90.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -120.0000 88

 80 omega   26.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000    0.0000 -150.0000 152

 81 omega   83.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   69.0000  116.1999 95

 82 omega   26.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000    0.0000 -180.0000 152

 83 omega   89.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -30.0000 89

 84 omega   88.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   47.0000    2.4272 90

 85 omega   26.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000    0.0000 -120.0000 152

 86 omega   26.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000    0.0000  -90.0000 152

 87 omega   26.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000    0.0000  -60.0000 152

 88 omega   90.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   38.0000  136.9449 88

 89 omega   90.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  -30.0000 88

 90 omega   41.00   99.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -30.0000 58
;
_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      -0.1518784000
_diffrn_orient_matrix_UB_12      -0.0915879000
_diffrn_orient_matrix_UB_13      -0.0389946000
_diffrn_orient_matrix_UB_21      0.0248406000
_diffrn_orient_matrix_UB_22      -0.0554907000
_diffrn_orient_matrix_UB_23      0.0955412000
_diffrn_orient_matrix_UB_31      -0.0528806000
_diffrn_orient_matrix_UB_32      0.1003746000
_diffrn_orient_matrix_UB_33      0.0547790000
_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  0.0278
_diffrn_reflns_av_unetI/netI     0.0102
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            83630
_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         71.952
_diffrn_reflns_theta_min         3.352
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.933
_exptl_absorpt_correction_T_max  0.678
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.584
_exptl_crystal_description       fragment
_exptl_crystal_F_000             689
_exptl_crystal_size_max          0.1705
_exptl_crystal_size_mid          0.1509
_exptl_crystal_size_min          0.0684
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.00036(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+1.5982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5571
_reflns_number_total             5695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma22_8
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_database_code               7041632
_chemical_oxdiff_formula         'C18 H20 Br3 F Si4'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelx_res_checksum              90144
_shelxl_version_number           2014-3