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_7041639
_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         'C33 H40 Si4'
_chemical_formula_sum            'C33 H40 Si4'
_chemical_formula_weight         549.01
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-27
_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                83.1033(10)
_cell_angle_beta                 82.0102(10)
_cell_angle_gamma                66.9065(14)
_cell_formula_units_Z            2
_cell_length_a                   10.57483(14)
_cell_length_b                   10.99150(16)
_cell_length_c                   16.03795(17)
_cell_measurement_reflns_used    40440
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.1900
_cell_measurement_theta_min      2.7680
_cell_volume                     1693.71(4)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9885
_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    -59.00  33.00   1.00    5.00    --  -38.50  38.00  90.00   92
  2  \w   -110.00  -8.00   1.00    5.00    --  -38.50 -77.00-180.00  102
  3  \w    -64.00  30.00   1.00    5.00    --  -38.50  57.00 -90.00   94
  4  \w     13.00 114.00   1.00    5.00    --   42.95  77.00  60.00  101
  5  \w     13.00 114.00   1.00    5.00    --   42.95  77.00-150.00  101
  6  \w     57.00 126.00   1.00    5.00    --   42.95 178.00  90.00   69
  7  \w      1.00  82.00   1.00    5.00    --   42.95 -99.00 150.00   81
  8  \w     18.00 111.00   1.00    5.00    --   42.95  57.00 -30.00   93
  9  \w     22.00 114.00   1.00    5.00    --   42.95  38.00 120.00   92
 10  \w     13.00 114.00   1.00    5.00    --   42.95  77.00   0.00  101
 11  \w     18.00 111.00   1.00    5.00    --   42.95  57.00-120.00   93
 12  \w     13.00 114.00   1.00    5.00    --   42.95  77.00 -90.00  101
 13  \w     13.00 114.00   1.00    5.00    --   42.95  77.00 120.00  101
 14  \w     31.00 109.00   1.00    5.00    --  111.00 -94.00-120.00   78
 15  \w     85.00 178.00   1.00    5.00    --  111.00  61.00  30.00   93
 16  \w     81.00 178.00   1.00    5.00    --  111.00  77.00 120.00   97
 17  \w     81.00 178.00   1.00    5.00    --  111.00  77.00-180.00   97
 18  \w     81.00 178.00   1.00    5.00    --  111.00  77.00-150.00   97
 19  \w     41.00 122.00   1.00    5.00    --  111.00-125.00-120.00   81
 20  \w     41.00 122.00   1.00    5.00    --  111.00-125.00  60.00   81
 21  \w     83.00 178.00   1.00    5.00    --  111.00  67.00  40.83   95
 22  \w     89.00 178.00   1.00    5.00    --  111.00  45.00-120.00   89
 23  \w     81.00 178.00   1.00    5.00    --  111.00  77.00 -90.00   97
 24  \w     41.00 122.00   1.00    5.00    --  111.00-125.00 150.00   81
 25  \w     81.00 178.00   1.00    5.00    --  111.00  77.00 -60.00   97
 26  \w     85.00 178.00   1.00    5.00    --  111.00  61.00-150.00   93
 27  \w     81.00 178.00   1.00    5.00    --  111.00  77.00-120.00   97
 28  \w     85.00 178.00   1.00    5.00    --  111.00  61.00 150.00   93
 29  \w     81.00 178.00   1.00    5.00    --  111.00  77.00   0.00   97
 30  \w     85.00 178.00   1.00    5.00    --  111.00  61.00  90.00   93
 31  \w     85.00 178.00   1.00    5.00    --  111.00  61.00 120.00   93
 32  \w     81.00 178.00   1.00    5.00    --  111.00  77.00 150.00   97
 33  \w     85.00 178.00   1.00    5.00    --  111.00  61.00 -60.00   93
 34  \w     85.00 178.00   1.00    5.00    --  111.00  61.00   0.00   93
 35  \w     81.00 178.00   1.00    5.00    --  111.00  77.00  60.00   97
 36  \w     85.00 178.00   1.00    5.00    --  111.00  61.00 -30.00   93
 37  \w     81.00 178.00   1.00    5.00    --  111.00  77.00  90.00   97
 38  \w     85.00 178.00   1.00    5.00    --  111.00  61.00-120.00   93
 39  \w     40.00 141.00   1.00    5.00    --  111.00 -77.00  60.00  101
 40  \w     85.00 178.00   1.00    5.00    --  111.00  61.00 -90.00   93
 41  \w     89.00 178.00   1.00    5.00    --  111.00  45.00 -30.00   89
 42  \w     31.00 109.00   1.00    5.00    --  111.00 -94.00 -90.00   78
 43  \w     81.00 178.00   1.00    5.00    --  111.00  77.00 -30.00   97
 44  \w     40.00 141.00   1.00    5.00    --  111.00 -77.00 -60.00  101
 45  \w     89.00 178.00   1.00    5.00    --  111.00  45.00  60.00   89
 46  \w     85.00 178.00   1.00    5.00    --  111.00  61.00  60.00   93
 47  \w     85.00 178.00   1.00    5.00    --  111.00  61.00-180.00   93
 48  \w     83.00 178.00   1.00    5.00    --  111.00  68.00 167.36   95
 49  \w     85.00 178.00   1.00    5.00    --  111.00  62.00-111.89   93
 50  \w   -124.00  47.00   1.00    5.00    --  -38.50   0.00-180.00  171
 51  \w   -107.00 -13.00   1.00    5.00    --  -38.50 -57.00 -60.00   94
 52  \w   -124.00  47.00   1.00    5.00    --  -38.50   0.00-120.00  171
 53  \w   -124.00  47.00   1.00    5.00    --  -38.50   0.00-150.00  171
 54  \w   -124.00  -3.00   1.00    5.00    --  -38.50   0.00 -90.00  121
 55  \w     57.00 126.00   1.00    5.00    --   42.95 178.00 -60.00   69
 56  \w     13.00 114.00   1.00    5.00    --   42.95  77.00-180.00  101
 57  \w     22.00 114.00   1.00    5.00    --   42.95  38.00   0.00   92
 58  \w     18.00 111.00   1.00    5.00    --   42.95  57.00   0.00   93
 59  \w     13.00 114.00   1.00    5.00    --   42.95  77.00  90.00  101
 60  \w     18.00 111.00   1.00    5.00    --   42.95  57.00  30.00   93
 61  \w     18.00 111.00   1.00    5.00    --   42.95  57.00-180.00   93
 62  \w     22.00 114.00   1.00    5.00    --   42.95  38.00 -30.00   92
;
_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      0.0383365000
_diffrn_orient_matrix_UB_12      -0.1507312000
_diffrn_orient_matrix_UB_13      0.0022504000
_diffrn_orient_matrix_UB_21      0.0328542000
_diffrn_orient_matrix_UB_22      0.0049941000
_diffrn_orient_matrix_UB_23      -0.0966935000
_diffrn_orient_matrix_UB_31      0.1509620000
_diffrn_orient_matrix_UB_32      -0.0243406000
_diffrn_orient_matrix_UB_33      0.0101528000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0100
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            61286
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.996
_diffrn_reflns_theta_min         2.789
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.756
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.724
_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    1.077
_exptl_crystal_description       fragment
_exptl_crystal_F_000             588.000
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0462P)^2^+0.8716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6491
_reflns_number_total             6651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma38_10
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_database_code               7041639
_chemical_oxdiff_formula         'C33 H40 Si4'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.334
_oxdiff_exptl_absorpt_empirical_full_min 0.857
_shelx_res_checksum              51379
_shelxl_version_number           2014-3