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_7041636
_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 H33 F Si4'
_chemical_formula_sum            'C24 H33 F Si4'
_chemical_formula_weight         452.86
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-23
_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                 105.035(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.3989(4)
_cell_length_b                   13.8715(3)
_cell_length_c                   21.2423(5)
_cell_measurement_reflns_used    75694
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      27.8190
_cell_measurement_theta_min      1.8510
_cell_volume                     5235.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9495
_diffrn_measurement_details
;
  1 omega    2.00   74.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989 -125.0000  -52.8226 72

  2 omega  -53.00   38.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989  -57.0000  150.0000 91

  3 omega  -14.00   86.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989   77.0000   30.0000 100

  4 omega   -5.00   85.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989   57.0000  150.0000 90

  5 omega  -53.00   38.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989  -57.0000    0.0000 91

  6 omega  -14.00   86.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989   77.0000 -120.0000 100

  7 omega  -28.00   89.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989   19.0000    0.0000 117

  8 omega  -38.00   52.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -      -16.3771   57.0000  -90.0000 90

  9 omega  -78.00   -6.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -      -16.3771  131.0000    1.9200 72

 10 omega   -5.00   85.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989   57.0000    0.0000 90

 11 omega    4.00   76.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989 -128.0000   54.4389 72

 12 omega   35.00   92.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989  178.0000 -180.0000 57

 13 omega  -53.00   38.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989  -57.0000  -90.0000 91

 14 omega  -83.00  -10.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -      -16.3771  139.0000  114.6111 73

 15 omega  -84.00  -11.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -      -16.3771  141.0000   88.0319 73

 16 omega  -20.00   26.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -      -16.3771  -99.0000 -120.0000 46

 17 omega  -53.00   38.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989  -57.0000  -60.0000 91

 18 omega  -57.00   27.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -       16.2989    0.0000 -180.0000 84

 19 omega  -85.00    5.00   1.0000    9.3400
omega____ theta____ kappa____ phi______ frames
    -      -16.3771  -57.0000   30.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0287328000
_diffrn_orient_matrix_UB_12      0.0346238000
_diffrn_orient_matrix_UB_13      0.0115550000
_diffrn_orient_matrix_UB_21      -0.0276140000
_diffrn_orient_matrix_UB_22      0.0346960000
_diffrn_orient_matrix_UB_23      0.0020781000
_diffrn_orient_matrix_UB_31      0.0025496000
_diffrn_orient_matrix_UB_32      -0.0145325000
_diffrn_orient_matrix_UB_33      0.0325014000
_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  0.0411
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            155423
_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         27.000
_diffrn_reflns_theta_min         1.700
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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    1.149
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.6848
_exptl_crystal_size_mid          0.4239
_exptl_crystal_size_min          0.1424
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         11387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0604P)^2^+1.7027P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10247
_reflns_number_total             11387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma17_5
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_database_code               7041636
_chemical_oxdiff_formula         'C24 H13 F Si4'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelx_res_checksum              47838
_shelxl_version_number           2013-2