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_7041634
_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         'C18 H12 Bi F Si'
_chemical_formula_sum            'C18 H12 Bi F Si'
_chemical_formula_weight         484.35
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-22
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.56012(16)
_cell_length_b                   8.59306(18)
_cell_length_c                   21.6023(5)
_cell_measurement_reflns_used    30177
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      29.9460
_cell_measurement_theta_min      2.5470
_cell_volume                     1589.01(6)
_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      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9979
_diffrn_measured_fraction_theta_max 0.9938
_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    -47.00  54.00   1.00    7.50    --  -17.00  77.00  30.00  101
  2  \w    -13.00  89.00   1.00    7.50    --   17.39  77.00 150.00  102
  3  \w    -54.00  -5.00   1.00    7.50    --   17.39 -38.00-180.00   49
  4  \w    -75.00  -2.00   1.00    7.50    --   -9.70 -57.00   0.00   73
  5  \w    -19.00  49.00   1.00    7.50    --   10.09 -99.00   0.00   68
  6  \w    -24.00  40.00   1.00    7.50    --   10.09 -77.00-120.00   64
  7  \w    -55.00  -3.00   1.00    7.50    --   10.09 -77.00 150.00   52
  8  \w      1.00  40.00   1.00    7.50    --   10.09 -77.00 150.00   39
  9  \w      7.00  76.00   1.00    7.50    --   10.09  77.00 -90.00   69
 10  \w    -20.00  29.00   1.00    7.50    --   -9.70 -99.00-180.00   49
 11  \w    -35.00  59.00   1.00    7.50    --   -9.70  57.00 -60.00   94
 12  \w    -81.00  11.00   1.00    7.50    --   -9.70 -38.00-120.00   92
 13  \w    -15.00  78.00   1.00    7.50    --   10.09  57.00  60.00   93
 14  \w    -20.00  49.00   1.00    7.50    --   10.09 -99.00-180.00   69
 15  \w    -20.00  49.00   1.00    7.50    --   10.09 -99.00-150.00   69
 16  \w      8.00  70.00   1.00    7.50    --   10.09-135.00 -33.00   62
 17  \w    -95.00  -2.00   1.00    7.50    --   -9.70   0.00-180.00   93
;
_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      -0.0089163000
_diffrn_orient_matrix_UB_12      -0.0168129000
_diffrn_orient_matrix_UB_13      0.0319399000
_diffrn_orient_matrix_UB_21      -0.0445517000
_diffrn_orient_matrix_UB_22      -0.0669836000
_diffrn_orient_matrix_UB_23      -0.0075283000
_diffrn_orient_matrix_UB_31      0.0692991000
_diffrn_orient_matrix_UB_32      -0.0452245000
_diffrn_orient_matrix_UB_33      -0.0007382000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            57635
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.996
_diffrn_reflns_theta_min         2.551
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.171
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.588
_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    2.025
_exptl_crystal_description       fragment
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.039
_refine_diff_density_max         1.941
_refine_diff_density_min         -1.908
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Flack x determined using 1844 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.033(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         4589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+1.7749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0528
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                4447
_reflns_number_total             4589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma47_mo_4
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_database_code               7041634
_chemical_oxdiff_formula         'C18 H12 Bi F Si'
_chemical_oxdiff_usercomment     ' '
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 2.649
_oxdiff_exptl_absorpt_empirical_full_min 0.613
_shelx_res_checksum              61715
_shelxl_version_number           2014-3