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_7041631
_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 Cl3 F Si4'
_chemical_formula_sum            'C24 H30 Cl3 F Si4'
_chemical_formula_weight         556.19
_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   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                102.500(9)
_cell_angle_beta                 91.619(9)
_cell_angle_gamma                97.127(10)
_cell_formula_units_Z            2
_cell_length_a                   8.8156(11)
_cell_length_b                   9.6417(12)
_cell_length_c                   17.3878(16)
_cell_measurement_reflns_used    11737
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.1650
_cell_measurement_theta_min      4.6950
_cell_volume                     1429.4(3)
_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      100.01(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 0.9854
_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   -102.00 -66.00   1.00    4.67    --  -38.50 -77.00   0.00   36
  2  \w    -55.00  33.00   1.00    4.67    --  -38.50  38.00  30.00   88
  3  \w    -85.00  -9.00   1.00    4.67    --  -38.50 -19.00-180.00   76
  4  \w    -35.00  -8.00   1.00    4.67    --  -38.50 -77.00   0.00   27
  5  \w     15.00  57.00   1.00    4.67    --   43.20  77.00 -30.00   42
  6  \w     28.00  59.00   1.00    4.67    --   43.20  38.00  30.00   31
  7  \w     15.00 114.00   1.00    4.67    --   43.20  77.00  90.00   99
  8  \w     85.00 113.00   1.00    4.67    --   43.20  38.00  30.00   28
  9  \w     11.00  38.00   1.00    4.67    --   43.20  84.00-106.60   27
 10  \w     13.00  66.00   1.00    4.67    --   43.20  77.00-180.00   53
 11  \w     57.00 126.00   1.00    4.67    --   43.20 178.00   0.00   69
 12  \w     62.00 109.00   1.00    4.67    --   43.20  57.00 -60.00   47
 13  \w     73.00 114.00   1.00    4.67    --   43.20  77.00 -30.00   41
 14  \w     58.00 127.00   1.00    4.67    --   43.20 178.00-180.00   69
 15  \w     20.00  60.00   1.00    4.67    --   43.20  57.00 -60.00   40
 16  \w     57.00 101.00   1.00    4.67    --   43.20 178.00 -90.00   44
 17  \w     18.00  51.00   1.00    4.67    --   43.20  57.00  60.00   33
 18  \w     62.00 108.00   1.00    4.67    --   43.20  57.00  60.00   46
 19  \w     46.00 120.00   1.00   18.68    --  111.00-125.00 120.00   74
 20  \w     95.00 122.00   1.00   18.68    --  111.00-125.00 -90.00   27
 21  \w     85.00 161.00   1.00   18.68    --  111.00  61.00-120.00   76
 22  \w    115.00 178.00   1.00   18.68    --  111.00  77.00  60.00   63
 23  \w     42.00  67.00   1.00   18.68    --  111.00-125.00   0.00   25
 24  \w     85.00 163.00   1.00   18.68    --  111.00  61.00 150.00   78
 25  \w     80.00 120.00   1.00   18.68    --  111.00-125.00   0.00   40
 26  \w     85.00 112.00   1.00   18.68    --  111.00  61.00  60.00   27
 27  \w     81.00 108.00   1.00   18.68    --  111.00  77.00  60.00   27
 28  \w     86.00 111.00   1.00   18.68    --  111.00  61.00   0.00   25
 29  \w     88.00 178.00   1.00   18.68    --  111.00  46.00-153.71   90
 30  \w     81.00 108.00   1.00   18.68    --  111.00  77.00 -60.00   27
 31  \w    137.00 162.00   1.00   18.68    --  111.00  61.00 120.00   25
 32  \w     85.00 132.00   1.00   18.68    --  111.00  61.00 120.00   47
 33  \w     58.00 141.00   1.00   18.68    --  111.00 -77.00-180.00   83
 34  \w     32.00  83.00   1.00   18.68    --  111.00 -94.00-180.00   51
 35  \w     81.00 108.00   1.00   18.68    --  111.00  77.00 -90.00   27
 36  \w     85.00 111.00   1.00   18.68    --  111.00  61.00-180.00   26
 37  \w     84.00 178.00   1.00   18.68    --  111.00  68.00 -25.06   94
 38  \w    132.00 160.00   1.00   18.68    --  111.00  77.00-180.00   28
 39  \w     81.00 107.00   1.00   18.68    --  111.00  77.00-180.00   26
 40  \w     31.00 107.00   1.00   18.68    --  111.00 -94.00 120.00   76
 41  \w     86.00 112.00   1.00   18.68    --  111.00  61.00 -30.00   26
 42  \w     81.00 169.00   1.00   18.68    --  111.00  77.00 120.00   88
 43  \w     81.00 107.00   1.00   18.68    --  111.00  77.00  30.00   26
 44  \w     81.00 107.00   1.00   18.68    --  111.00  77.00  90.00   26
 45  \w     81.00 108.00   1.00   18.68    --  111.00  77.00 150.00   27
 46  \w    137.00 175.00   1.00   18.68    --  111.00  77.00 150.00   38
 47  \w     82.00 130.00   1.00   18.68    --  111.00  77.00   0.00   48
 48  \w     85.00 112.00   1.00   18.68    --  111.00  61.00 -60.00   27
 49  \w     89.00 116.00   1.00   18.68    --  111.00  45.00  90.00   27
 50  \w     85.00 177.00   1.00   18.68    --  111.00  61.00 -90.00   92
 51  \w     81.00 107.00   1.00   18.68    --  111.00  77.00 -30.00   26
 52  \w     91.00 135.00   1.00   18.68    --  111.00  45.00-120.00   44
 53  \w     81.00 107.00   1.00   18.68    --  111.00  77.00-120.00   26
 54  \w     41.00  74.00   1.00   18.68    --  111.00-125.00 -90.00   33
 55  \w    129.00 157.00   1.00   18.68    --  111.00  61.00  90.00   28
 56  \w     85.00 111.00   1.00   18.68    --  111.00  61.00  90.00   26
 57  \w     44.00 136.00   1.00   18.68    --  111.00 -61.00 -60.00   92
 58  \w     85.00 178.00   1.00   18.68    --  111.00  61.00  30.00   93
 59  \w     87.00 177.00   1.00   18.68    --  111.00  53.00 -43.68   90
 60  \w     83.00 109.00   1.00   18.68    --  111.00  67.00-148.07   26
;
_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      0.0627668000
_diffrn_orient_matrix_UB_12      0.0550688000
_diffrn_orient_matrix_UB_13      -0.0711252000
_diffrn_orient_matrix_UB_21      0.1212490000
_diffrn_orient_matrix_UB_22      -0.1036715000
_diffrn_orient_matrix_UB_23      -0.0072499000
_diffrn_orient_matrix_UB_31      -0.1114280000
_diffrn_orient_matrix_UB_32      -0.1159724000
_diffrn_orient_matrix_UB_33      -0.0559565000
_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  0.0404
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25090
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.993
_diffrn_reflns_theta_min         2.607
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.656
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67042
_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    1.289
_exptl_crystal_description       plate
_exptl_crystal_F_000             580.0
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.724
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5612
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0541P)^2^+0.8390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4877
_reflns_number_total             5612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma42_7
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_database_code               7041631
_chemical_oxdiff_formula         'C24 H30 Cl3 F Si4'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.459
_oxdiff_exptl_absorpt_empirical_full_min 0.748
_shelx_res_checksum              78715
_shelxl_version_number           2014-3