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_7041633
_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         'C24 H30 F4 Si4'
_chemical_formula_sum            'C24 H30 F4 Si4'
_chemical_formula_weight         506.84
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-29
_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                90
_cell_angle_beta                 91.508(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1783(10)
_cell_length_b                   9.5489(3)
_cell_length_c                   30.1357(13)
_cell_measurement_reflns_used    41392
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.1630
_cell_measurement_theta_min      2.8940
_cell_volume                     5229.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9981
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -122.00 -35.00   1.00    1.67    --  -38.50-178.00 120.00   87
  2  \w    -64.00  30.00   1.00    1.67    --  -38.50  57.00   0.00   94
  3  \w     24.00  52.00   1.00    1.67    --   42.95  38.00 -30.00   28
  4  \w     25.00  63.00   1.00    1.67    --   42.95  77.00-180.00   38
  5  \w     56.00  88.00   1.00    1.67    --   42.95  77.00  30.00   32
  6  \w     13.00 113.00   1.00    1.67    --   42.95  77.00-120.00  100
  7  \w     57.00 126.00   1.00    1.67    --   42.95 178.00-180.00   69
  8  \w     14.00  72.00   1.00    1.67    --   42.95  77.00 150.00   58
  9  \w     69.00 113.00   1.00    1.67    --   42.95  77.00  90.00   44
 10  \w     61.00 114.00   1.00    1.67    --   42.95  77.00 -90.00   53
 11  \w     18.00 104.00   1.00    1.67    --   42.95  57.00  90.00   86
 12  \w     72.00 111.00   1.00    1.67    --   42.95  77.00 -60.00   39
 13  \w     58.00 126.00   1.00    1.67    --   42.95 178.00 -90.00   68
 14  \w     22.00  99.00   1.00    1.67    --   42.95  38.00-120.00   77
 15  \w     14.00  64.00   1.00    1.67    --   42.95  77.00 -60.00   50
 16  \w     13.00  47.00   1.00    1.67    --   42.95  77.00  30.00   34
 17  \w     18.00 105.00   1.00    1.67    --   42.95  57.00   0.00   87
 18  \w     20.00  53.00   1.00    1.67    --   42.95  77.00 -90.00   33
 19  \w     14.00  50.00   1.00    1.67    --   42.95  77.00  90.00   36
 20  \w     83.00 161.00   1.00    6.67    --  111.00  70.00  24.42   78
 21  \w     85.00 118.00   1.00    6.67    --  111.00  61.00 -61.44   33
 22  \w     85.00 177.00   1.00    6.67    --  111.00  61.00 -92.31   92
 23  \w     81.00 107.00   1.00    6.67    --  111.00  77.00-120.00   26
 24  \w    128.00 173.00   1.00    6.67    --  111.00  64.00   4.10   45
 25  \w     32.00 106.00   1.00    6.67    --  111.00 -94.00  30.00   74
 26  \w     35.00 108.00   1.00    6.67    --  111.00 -94.00-180.00   73
 27  \w     81.00 108.00   1.00    6.67    --  111.00  77.00   0.00   27
 28  \w     81.00 107.00   1.00    6.67    --  111.00  77.00-150.00   26
 29  \w     42.00 122.00   1.00    6.67    --  111.00-125.00  30.00   80
 30  \w     48.00 136.00   1.00    6.67    --  111.00 -61.00  30.00   88
 31  \w     41.00 141.00   1.00    6.67    --  111.00 -77.00-150.00  100
 32  \w     84.00 127.00   1.00    6.67    --  111.00  64.00   4.10   43
 33  \w     84.00 110.00   1.00    6.67    --  111.00  64.00 -74.64   26
 34  \w     85.00 147.00   1.00    6.67    --  111.00  59.00  68.13   62
 35  \w     97.00 122.00   1.00    6.67    --  111.00-125.00 -30.00   25
 36  \w     85.00 111.00   1.00    6.67    --  111.00  61.00  60.00   26
 37  \w     82.00 108.00   1.00    6.67    --  111.00  74.00  59.45   26
 38  \w     85.00 111.00   1.00    6.67    --  111.00  61.00   0.00   26
 39  \w     91.00 122.00   1.00    6.67    --  111.00-125.00 150.00   31
 40  \w     83.00 109.00   1.00    6.67    --  111.00  70.00-123.48   26
 41  \w     83.00 163.00   1.00    6.67    --  111.00  67.00 -56.79   80
 42  \w     84.00 178.00   1.00    6.67    --  111.00  63.00-142.70   94
 43  \w     85.00 111.00   1.00    6.67    --  111.00  61.00 120.00   26
 44  \w     43.00  81.00   1.00    6.67    --  111.00-125.00 -30.00   38
 45  \w     81.00 107.00   1.00    6.67    --  111.00  77.00 -60.00   26
 46  \w     85.00 112.00   1.00    6.67    --  111.00  61.00 150.00   27
 47  \w     81.00 108.00   1.00    6.67    --  111.00  77.00-180.00   27
 48  \w    119.00 176.00   1.00    6.67    --  111.00  77.00-180.00   57
 49  \w     81.00 108.00   1.00    6.67    --  111.00  77.00 150.00   27
 50  \w     85.00 178.00   1.00    6.67    --  111.00  61.00-120.00   93
 51  \w     86.00 177.00   1.00    6.67    --  111.00  55.00 133.62   91
 52  \w     81.00 172.00   1.00    6.67    --  111.00  77.00  90.00   91
 53  \w     89.00 115.00   1.00    6.67    --  111.00  45.00-150.00   26
 54  \w     81.00 107.00   1.00    6.67    --  111.00  77.00 120.00   26
 55  \w     81.00 177.00   1.00    6.67    --  111.00  77.00  30.00   96
 56  \w     83.00 109.00   1.00    6.67    --  111.00  69.00  21.03   26
 57  \w     82.00 144.00   1.00    6.67    --  111.00  72.00  85.69   62
 58  \w     85.00 111.00   1.00    6.67    --  111.00  61.00-180.00   26
 59  \w     82.00 108.00   1.00    6.67    --  111.00  74.00 145.65   26
 60  \w     81.00 130.00   1.00    6.67    --  111.00  77.00 -30.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0835443000
_diffrn_orient_matrix_UB_12      -0.0023762000
_diffrn_orient_matrix_UB_13      0.0073445000
_diffrn_orient_matrix_UB_21      -0.0098914000
_diffrn_orient_matrix_UB_22      0.1280061000
_diffrn_orient_matrix_UB_23      -0.0306461000
_diffrn_orient_matrix_UB_31      -0.0108167000
_diffrn_orient_matrix_UB_32      -0.0979482000
_diffrn_orient_matrix_UB_33      -0.0402022000
_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  0.0704
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            93632
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.989
_diffrn_reflns_theta_min         2.934
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.455
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.30a (Agilent, 2015)
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    1.288
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.355
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0851
_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^)+(0.1072P)^2^+29.5396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2280
_refine_ls_wR_factor_ref         0.2305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8885
_reflns_number_total             9331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma41_6
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_database_code               7041633
_chemical_oxdiff_formula         'C24 H30 F4 Si4'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     43.60
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.458
_oxdiff_exptl_absorpt_empirical_full_min 0.624
_shelx_res_checksum              49629
_shelxl_version_number           2014-3