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_7041640
_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 Br3 F Si'
_chemical_formula_sum            'C18 H12 Br3 F Si'
_chemical_formula_weight         515.10
_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             2016-05-19
_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                105.9021(13)
_cell_angle_beta                 99.9179(12)
_cell_angle_gamma                95.7928(12)
_cell_formula_units_Z            4
_cell_length_a                   8.52630(12)
_cell_length_b                   14.8043(2)
_cell_length_c                   15.1065(2)
_cell_measurement_reflns_used    28573
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      30.0060
_cell_measurement_theta_min      2.3070
_cell_volume                     1784.24(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 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(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     34.00 100.00   1.00   17.00    --   25.04-178.00  60.00   66
  2  \w    -20.00  66.00   1.00   17.00    --   25.04 -99.00-180.00   86
  3  \w    -20.00  66.00   1.00   17.00    --   25.04 -99.00 -60.00   86
  4  \w      3.00  96.00   1.00   17.00    --   25.04  38.00-150.00   93
  5  \w      7.00  93.00   1.00   17.00    --   25.04  57.00   0.00   86
  6  \w    -20.00  66.00   1.00   17.00    --   25.04 -99.00  60.00   86
  7  \w     -4.00  94.00   1.00   17.00    --   25.04  77.00  90.00   98
  8  \w    -46.00  47.00   1.00   17.00    --   25.04 -38.00  90.00   93
  9  \w     -4.00  94.00   1.00   17.00    --   25.04  77.00-120.00   98
 10  \w    -47.00  63.00   1.00   17.00    --   25.04 -19.00-180.00  110
 11  \w    -97.00 -35.00   1.00   17.00    --  -23.50-178.00 150.00   62
 12  \w    -95.00  48.00   1.00   17.00    --  -23.50   0.00-180.00  143
 13  \w     35.00  99.00   1.00   17.00    --   25.04 178.00-180.00   64
 14  \w     -4.00  94.00   1.00   17.00    --   25.04  77.00 150.00   98
 15  \w      7.00  93.00   1.00   17.00    --   25.04  57.00 -60.00   86
 16  \w      1.00  79.00   1.00   17.00    --   25.04-124.00  50.00   78
 17  \w     -4.00  94.00   1.00   17.00    --   25.04  77.00   0.00   98
 18  \w      7.00  93.00   1.00   17.00    --   25.04  57.00-150.00   86
 19  \w    -95.00  48.00   1.00   17.00    --  -23.50   0.00-120.00  143
 20  \w    -95.00  48.00   1.00   17.00    --  -23.50   0.00 -90.00  143
 21  \w    -95.00 -39.00   1.00   17.00    --  -23.50   0.00 -60.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0818512000
_diffrn_orient_matrix_UB_12      -0.0053178000
_diffrn_orient_matrix_UB_13      0.0004266000
_diffrn_orient_matrix_UB_21      -0.0155082000
_diffrn_orient_matrix_UB_22      -0.0107139000
_diffrn_orient_matrix_UB_23      -0.0497223000
_diffrn_orient_matrix_UB_31      0.0192534000
_diffrn_orient_matrix_UB_32      0.0489997000
_diffrn_orient_matrix_UB_33      0.0044533000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            85951
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.081
_diffrn_reflns_theta_min         1.708
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.855
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 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    1.918
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         10469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0264P)^2^+1.5733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8916
_reflns_number_total             10469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma51_3
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_database_code               7041640
_chemical_oxdiff_formula         'C18 H12 Br3 F Si'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_date_sample_data_collection 2016-05-18
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24),
  C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36)
;
_olex2_submission_special_instructions 'No special instructions were received'
_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 1.431
_oxdiff_exptl_absorpt_empirical_full_min 0.797
_shelx_shelxl_version_number     2014/7