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_7041630
_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 H15 F Si'
_chemical_formula_sum            'C24 H15 F Si'
_chemical_formula_weight         350.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-20
_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                 92.003(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3691(3)
_cell_length_b                   15.3606(6)
_cell_length_c                   12.4364(4)
_cell_measurement_reflns_used    3084
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.9450
_cell_measurement_theta_min      4.5550
_cell_volume                     1788.69(11)
_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 1.0000
_diffrn_measured_fraction_theta_max 0.9806
_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 -13.00   1.00   30.00    --  -38.50 -57.00-120.00   89
  2  \w   -109.00 -20.00   1.00   30.00    --  -38.50 -38.00  60.00   89
  3  \w    -90.00 -15.00   1.00   30.00    --  -38.50 -57.00 -30.00   75
  4  \w   -121.00 -92.00   1.00   30.00    --  -38.50 178.00-150.00   29
  5  \w    -28.00  44.00   1.00   30.00    --   42.95 -38.00-180.00   72
  6  \w     86.00 124.00   1.00   30.00    --   42.95 178.00 -90.00   38
  7  \w     98.00 165.00   1.00  120.00    --  109.03 125.00  90.00   67
  8  \w     55.00 126.00   1.00  120.00    --  109.03 -30.00  60.00   71
  9  \w     88.00 178.00   1.00  120.00    --  109.03  30.00-180.00   90
 10  \w     41.00  95.00   1.00  120.00    --  109.03 -45.00 -60.00   54
 11  \w    106.00 175.00   1.00  120.00    --  109.03  45.00-120.00   69
 12  \w     93.00 151.00   1.00  120.00    --  109.03  30.00 120.00   58
 13  \w     64.00 112.00   1.00  120.00    --  109.03 -30.00 -30.00   48
 14  \w     79.00 120.00   1.00  120.00    --  109.03-125.00  30.00   41
 15  \w     38.00  86.00   1.00  120.00    --  109.03 -94.00-150.00   48
 16  \w     89.00 118.00   1.00  120.00    --  109.03-125.00-120.00   29
 17  \w    121.00 177.00   1.00  120.00    --  109.03 125.00  30.00   56
 18  \w     96.00 144.00   1.00  120.00    --  109.03 125.00-120.00   48
 19  \w     38.00 138.00   1.00  120.00    --  109.03 -77.00  30.00  100
;
_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      -0.1431302000
_diffrn_orient_matrix_UB_12      -0.0273787000
_diffrn_orient_matrix_UB_13      0.0471411000
_diffrn_orient_matrix_UB_21      -0.0474724000
_diffrn_orient_matrix_UB_22      0.0959626000
_diffrn_orient_matrix_UB_23      0.0016644000
_diffrn_orient_matrix_UB_31      -0.0657048000
_diffrn_orient_matrix_UB_32      -0.0097702000
_diffrn_orient_matrix_UB_33      -0.1146881000
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12556
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.141
_diffrn_reflns_theta_min         4.576
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.666
_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    1.301
_exptl_crystal_description       plate
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.017
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0431P)^2^+0.5803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2780
_reflns_number_total             3631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma37_12
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_original_cell_volume        1788.70(10)
_cod_database_code               7041630
_chemical_oxdiff_formula         'c6 h6 Cl f si'
_chemical_oxdiff_usercomment     'C40 H34 Si3'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.302
_oxdiff_exptl_absorpt_empirical_full_min 0.713
_shelx_res_checksum              90781
_shelxl_version_number           2014-3