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_7041625
_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
'1.13(C20.49 H18.79 Si0.85), 0.25(C3.51 H3.07 Si0.15)'
_chemical_formula_sum            'C24 H21.96 Si'
_chemical_formula_weight         338.47
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_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                120
_cell_formula_units_Z            24
_cell_length_a                   23.2777(10)
_cell_length_b                   23.2777(10)
_cell_length_c                   25.4877(6)
_cell_measurement_reflns_used    12792
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.0430
_cell_measurement_theta_min      2.7560
_cell_volume                     11960.3(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega -122.00  -35.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  178.0000 -120.0000 87

  2 omega  -46.00   23.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -60.0000 69

  3 omega -114.00   -5.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000  -90.0000 109

  4 omega  -50.00   32.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   90.0000 82

  5 omega   23.00   53.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   57.0000    0.0000 30

  6 omega   15.00   78.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000  -60.0000 63

  7 omega   91.00  117.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.9488  178.0000  150.0000 26

  8 omega   18.00   78.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000  120.0000 60

  9 omega   57.00  126.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.9488  178.0000  -90.0000 69

 10 omega   22.00   86.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   38.0000 -180.0000 64

 11 omega   23.00  102.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   38.0000   60.0000 79

 12 omega   70.00  114.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000    0.0000 44

 13 omega   13.00   91.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000 -180.0000 78

 14 omega   14.00   68.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000 -120.0000 54

 15 omega   14.00   50.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000    0.0000 36

 16 omega   14.00   93.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.9488   77.0000   60.0000 79

 17 omega   33.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 32

 18 omega   97.00  122.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  150.0000 25

 19 omega   86.00  123.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   55.0000  -43.4289 37

 20 omega   82.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 93

 21 omega   81.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 26

 22 omega   85.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 26

 23 omega  117.00  152.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   72.0000  107.1996 35

 24 omega   85.00  132.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 47

 25 omega   81.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 27

 26 omega   47.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  150.0000 27

 27 omega   85.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 26

 28 omega   81.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   75.0000 -100.4557 26

 29 omega   85.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 30

 30 omega  122.00  149.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 27

 31 omega   86.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 91

 32 omega   81.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 26

 33 omega   81.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 97

 34 omega   85.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 31

 35 omega   81.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 28

 36 omega   41.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 76

 37 omega   82.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   72.0000  107.1996 29

 38 omega   81.00  173.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 92

 39 omega   40.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 69

 40 omega   81.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 26

 41 omega   81.00  173.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 92

 42 omega   84.00  140.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -120.0000 56

 43 omega   41.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -120.0000 42

 44 omega  113.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 65

 45 omega   85.00  161.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 76

 46 omega   81.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 26

 47 omega   45.00  141.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000   30.0000 96

 48 omega  124.00  176.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 52

 49 omega   89.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -180.0000 27

 50 omega   85.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 26

 51 omega   81.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 27

 52 omega   81.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 26

 53 omega  124.00  176.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 52

 54 omega   85.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 27

 55 omega   84.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 25

 56 omega   83.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   67.0000  144.0187 27

 57 omega   85.00  171.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   62.0000   39.2019 86

 58 omega   85.00  176.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   60.0000 -106.5288 91

 59 omega   83.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   69.0000 -148.6702 27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0007060000
_diffrn_orient_matrix_UB_12      0.0569677000
_diffrn_orient_matrix_UB_13      -0.0313892000
_diffrn_orient_matrix_UB_21      0.0137780000
_diffrn_orient_matrix_UB_22      -0.0269228000
_diffrn_orient_matrix_UB_23      -0.0507444000
_diffrn_orient_matrix_UB_31      -0.0752044000
_diffrn_orient_matrix_UB_32      -0.0429988000
_diffrn_orient_matrix_UB_33      -0.0095652000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            74800
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.883
_diffrn_reflns_theta_min         2.795
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.128
_exptl_crystal_description       cube
_exptl_crystal_F_000             4319
_exptl_crystal_size_max          0.037
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         5236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0872P)^2^+9.3585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3844
_reflns_number_total             5236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma31_18
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_original_cell_volume        11960.3(10)
_cod_database_code               7041625
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C24 H22 Si'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Si2B) = Uanis(Si2)
Uanis(C29A) = Uanis(C29B)
Uanis(Si1B) = Uanis(Si1A)
Uanis(C13A) = Uanis(C13B)
Uanis(C27A) = Uanis(C27B)
Uanis(C28A) = Uanis(C28B)
Uanis(C32A) = Uanis(C32B)
3. Others
 Sof(C1B)=Sof(C2B)=Sof(H2BA)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=
 Sof(H5B)=Sof(C6B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=1-FVAR(1)
 Sof(Si1B)=0.33333*(1-FVAR(2))
 Sof(Si1A)=Sof(H1A)=0.33333*FVAR(2)
 Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=FVAR(1)
 Sof(Si2B)=Sof(H2B)=Sof(C9B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11B)=Sof(C12B)=
 Sof(H12B)=Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=
 Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(C18B)=Sof(H18B)=Sof(C19B)=Sof(H19B)=
 Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21B)=Sof(C22B)=Sof(C23B)=Sof(H23B)=
 Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=
 Sof(H27B)=Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(H29B)=Sof(C30B)=Sof(C31B)=
 Sof(H31B)=Sof(C32B)=Sof(H32C)=Sof(H32D)=1-FVAR(2)
 Sof(Si2)=Sof(H2)=Sof(C9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=
 Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=
 Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(C23A)=Sof(H23A)=
 Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=
 Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(C31A)=
 Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C7A(H7A), C2B(H2BA), C3B(H3B),
 C4B(H4B), C5B(H5B), C7B(H7B), C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A),
 C15A(H15A), C18A(H18A), C19A(H19A), C20A(H20A), C21A(H21A), C23A(H23A),
 C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C31A(H31A), C10B(H10B),
 C11B(H11B), C12B(H12B), C13B(H13B), C15B(H15B), C18B(H18B), C19B(H19B),
 C20B(H20B), C21B(H21B), C23B(H23B), C26B(H26B), C27B(H27B), C28B(H28B),
 C29B(H29B), C31B(H31B)
4.b Fitted hexagon refined as free rotating group:
 C1B(C2B,C3B,C4B,C5B,C6B), C9A(C10A,C11A,C12A,C13A,C14A), C17A(C18A,C19A,C20A,
 C21A,C22A), C25A(C26A,C27A,C28A,C29A,C30A), C9B(C10B,C11B,C12B,C13B,C14B),
 C17B(C18B,C19B,C20B,C21B,C22B), C25B(C26B,C27B,C28B,C29B,C30B)
4.c X=CH2 refined with riding coordinates:
 C8A(H8AA,H8AB), C8B(H8BA,H8BB), C16A(H16A,H16B), C24A(H24A,H24B), C32A(H32A,
 H32B), C16B(H16C,H16D), C24B(H24C,H24D), C32B(H32C,H32D)
;
_olex2_date_sample_data_collection 1427735795.98
_olex2_date_sample_submission    1427151600
_olex2_submission_special_instructions 'No special instructions were received'