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_7041626
_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         'C27 H33 Cl6 F Si4'
_chemical_formula_sum            'C27 H33 Cl6 F Si4'
_chemical_formula_weight         701.59
_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             2015-04-15
_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                 98.2284(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.62445(7)
_cell_length_b                   16.09570(8)
_cell_length_c                   11.42592(5)
_cell_measurement_reflns_used    85905
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.2350
_cell_measurement_theta_min      3.5910
_cell_volume                     3389.93(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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9955
_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    -64.00  30.00   1.00    1.50    --  -38.50  57.00 -30.00   94
  2  \w   -110.00 -18.00   1.00    1.50    --  -38.50 -38.00-120.00   92
  3  \w     19.00 112.00   1.00    1.50    --   43.70  57.00-120.00   93
  4  \w     14.00 115.00   1.00    1.50    --   43.70  77.00 120.00  101
  5  \w     14.00 115.00   1.00    1.50    --   43.70  77.00 -90.00  101
  6  \w     14.00 115.00   1.00    1.50    --   43.70  77.00  60.00  101
  7  \w     57.00 127.00   1.00    1.50    --   43.70 178.00 -60.00   70
  8  \w     14.00 115.00   1.00    1.50    --   43.70  77.00 -30.00  101
  9  \w     57.00 127.00   1.00    1.50    --   43.70 178.00-150.00   70
 10  \w     23.00 115.00   1.00    1.50    --   43.70  38.00 -30.00   92
 11  \w     57.00 127.00   1.00    1.50    --   43.70 178.00 150.00   70
 12  \w     19.00 112.00   1.00    1.50    --   43.70  57.00  90.00   93
 13  \w     23.00 115.00   1.00    1.50    --   43.70  38.00  60.00   92
 14  \w     14.00 115.00   1.00    1.50    --   43.70  77.00-180.00  101
 15  \w     81.00 178.00   1.00    6.00    --  111.00  77.00 -60.00   97
 16  \w     31.00 109.00   1.00    6.00    --  111.00 -94.00-120.00   78
 17  \w     81.00 178.00   1.00    6.00    --  111.00  76.00 106.21   97
 18  \w     85.00 178.00   1.00    6.00    --  111.00  61.00  60.00   93
 19  \w     85.00 178.00   1.00    6.00    --  111.00  61.00-180.00   93
 20  \w     85.00 178.00   1.00    6.00    --  111.00  61.00 150.00   93
 21  \w     85.00 178.00   1.00    6.00    --  111.00  61.00  30.00   93
 22  \w     81.00 178.00   1.00    6.00    --  111.00  77.00 120.00   97
 23  \w     81.00 178.00   1.00    6.00    --  111.00  77.00  90.00   97
 24  \w     81.00 178.00   1.00    6.00    --  111.00  77.00-180.00   97
 25  \w     83.00 178.00   1.00    6.00    --  111.00  67.00-143.22   95
 26  \w     87.00 178.00   1.00    6.00    --  111.00  54.00  -9.19   91
 27  \w     43.00 137.00   1.00    6.00    --  111.00 -61.00  90.00   94
 28  \w     41.00 122.00   1.00    6.00    --  111.00-125.00-120.00   81
 29  \w     81.00 178.00   1.00    6.00    --  111.00  77.00  60.00   97
 30  \w     81.00 178.00   1.00    6.00    --  111.00  77.00 -90.00   97
 31  \w     81.00 178.00   1.00    6.00    --  111.00  77.00  30.00   97
 32  \w     81.00 178.00   1.00    6.00    --  111.00  77.00-150.00   97
 33  \w     40.00 141.00   1.00    6.00    --  111.00 -77.00 -90.00  101
 34  \w     85.00 178.00   1.00    6.00    --  111.00  61.00-150.00   93
 35  \w     85.00 178.00   1.00    6.00    --  111.00  61.00  90.00   93
 36  \w     31.00 109.00   1.00    6.00    --  111.00 -94.00  60.00   78
 37  \w     85.00 178.00   1.00    6.00    --  111.00  61.00 -30.00   93
 38  \w     81.00 178.00   1.00    6.00    --  111.00  77.00 -30.00   97
 39  \w     41.00 122.00   1.00    6.00    --  111.00-125.00 150.00   81
 40  \w     81.00 178.00   1.00    6.00    --  111.00  77.00   0.00   97
 41  \w     81.00 178.00   1.00    6.00    --  111.00  77.00-120.00   97
 42  \w     89.00 178.00   1.00    6.00    --  111.00  45.00 -60.00   89
 43  \w     85.00 178.00   1.00    6.00    --  111.00  61.00   0.00   93
 44  \w     81.00 178.00   1.00    6.00    --  111.00  77.00 150.00   97
 45  \w     85.00 178.00   1.00    6.00    --  111.00  61.00 -60.00   93
 46  \w     83.00 178.00   1.00    6.00    --  111.00  70.00-130.38   95
 47  \w     85.00 178.00   1.00    6.00    --  111.00  61.00 -90.00   93
 48  \w     41.00 122.00   1.00    6.00    --  111.00-125.00  30.00   81
 49  \w     83.00 178.00   1.00    6.00    --  111.00  68.00 126.77   95
 50  \w     87.00 178.00   1.00    6.00    --  111.00  54.00 106.08   91
 51  \w     85.00 178.00   1.00    6.00    --  111.00  61.00  42.16   93
 52  \w     83.00 178.00   1.00    6.00    --  111.00  67.00-152.43   95
 53  \w   -110.00  -8.00   1.00    1.50    --  -38.50 -77.00 -60.00  102
 54  \w   -122.00 -35.00   1.00    1.50    --  -38.50-178.00-180.00   87
 55  \w     23.00 115.00   1.00    1.50    --   43.70  38.00 150.00   92
 56  \w     23.00 115.00   1.00    1.50    --   43.70  38.00  90.00   92
 57  \w     19.00 112.00   1.00    1.50    --   43.70  57.00 -30.00   93
 58  \w     14.00 115.00   1.00    1.50    --   43.70  77.00-120.00  101
 59  \w     23.00 115.00   1.00    1.50    --   43.70  38.00-120.00   92
 60  \w     19.00 112.00   1.00    1.50    --   43.70  57.00-180.00   93
 61  \w     23.00 115.00   1.00    1.50    --   43.70  38.00-150.00   92
 62  \w     14.00 115.00   1.00    1.50    --   43.70  77.00   0.00  101
;
_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      -0.0774526000
_diffrn_orient_matrix_UB_12      -0.0048848000
_diffrn_orient_matrix_UB_13      0.0321461000
_diffrn_orient_matrix_UB_21      -0.0260097000
_diffrn_orient_matrix_UB_22      -0.0432698000
_diffrn_orient_matrix_UB_23      -0.1187576000
_diffrn_orient_matrix_UB_31      0.0176516000
_diffrn_orient_matrix_UB_32      -0.0852376000
_diffrn_orient_matrix_UB_33      0.0584573000
_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  0.0285
_diffrn_reflns_av_unetI/netI     0.0085
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            121594
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.548
_diffrn_reflns_theta_min         3.646
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.167
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.30a (Agilent, 2015)
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    1.375
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.129
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0328P)^2^+1.9109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6962
_reflns_number_total             7099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma34_20
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_database_code               7041626
_chemical_oxdiff_formula         'C27 H33 Cl6 F Si4'
_reflns_odcompleteness_completeness 99.97
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.202
_oxdiff_exptl_absorpt_empirical_full_min 0.847
_shelx_res_checksum              54894
_shelxl_version_number           2014-3