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_7041635
_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 H13 Br3 Si'
_chemical_formula_sum            'C18 H13 Br3 Si'
_chemical_formula_weight         497.10
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-01
_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                 92.952(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4821(4)
_cell_length_b                   7.8061(4)
_cell_length_c                   31.1863(14)
_cell_measurement_reflns_used    8725
_cell_measurement_temperature    99.8(4)
_cell_measurement_theta_max      29.9300
_cell_measurement_theta_min      2.6830
_cell_volume                     1819.05(16)
_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      99.98(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9945
_diffrn_measured_fraction_theta_max 0.9911
_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    -40.00  52.00   1.00   16.00    --  -17.00  48.00  73.40   92
  2  \w    -85.00   8.00   1.00   16.00    --  -17.00 -57.00-120.00   93
  3  \w    -90.00 -38.00   1.00   16.00    --  -17.00 153.00  70.54   52
  4  \w    -88.00   4.00   1.00   16.00    --  -17.00 -38.00  90.00   92
  5  \w    -75.00 -37.00   1.00   16.00    --  -17.00 131.00 175.15   38
;
_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      -0.0318454000
_diffrn_orient_matrix_UB_12      0.0851378000
_diffrn_orient_matrix_UB_13      0.0019083000
_diffrn_orient_matrix_UB_21      -0.0162732000
_diffrn_orient_matrix_UB_22      0.0040722000
_diffrn_orient_matrix_UB_23      -0.0225984000
_diffrn_orient_matrix_UB_31      -0.0879758000
_diffrn_orient_matrix_UB_32      -0.0315464000
_diffrn_orient_matrix_UB_33      0.0022424000
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            19343
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.690
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.712
_exptl_absorpt_correction_T_max  0.664
_exptl_absorpt_correction_T_min  0.497
_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    1.817
_exptl_crystal_description       fragment
_exptl_crystal_F_000             960.0
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         5267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0170P)^2^+0.7933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4427
_reflns_number_total             5267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma45_mo_2
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_original_cell_volume        1819.05(15)
_cod_database_code               7041635
_chemical_oxdiff_formula         'C18 H13 Br3 Si1'
_reflns_odcompleteness_completeness 99.45
_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 1.216
_oxdiff_exptl_absorpt_empirical_full_min 0.834
_shelx_res_checksum              97079
_shelxl_version_number           2014-3