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_7041627
_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 H39 F Si Sn3'
_chemical_formula_sum            'C33 H39 F Si Sn3'
_chemical_formula_weight         838.80
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-15
_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                 90.2126(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.80666(9)
_cell_length_b                   41.3809(2)
_cell_length_c                   13.17067(13)
_cell_measurement_reflns_used    129966
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.3080
_cell_measurement_theta_min      4.2250
_cell_volume                     6979.76(9)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9917
_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    -53.00  -6.00   1.00    4.67    --    6.00 131.00  14.89   47
  2  \w      0.00  26.00   1.00    4.67    --   38.00  94.00 -83.47   26
  3  \w   -121.00  -5.00   1.00    4.67    --  -42.33 -19.00-180.00  116
  4  \w   -115.00 -20.00   1.00    4.67    --  -42.33 -38.00  90.00   95
  5  \w   -112.00 -16.00   1.00    4.67    --  -42.33 -57.00 -60.00   96
  6  \w   -112.00 -16.00   1.00    4.67    --  -42.33 -57.00  60.00   96
  7  \w      1.00  82.00   1.00    4.67    --   42.33 -99.00  60.00   81
  8  \w      8.00  34.00   1.00    4.67    --   42.33  87.00 126.55   26
  9  \w     27.00 101.00   1.00    4.67    --   42.33-131.00 -43.00   74
 10  \w     13.00  40.00   1.00    4.67    --   46.00  83.00 -23.03   27
 11  \w     14.00  49.00   1.00    4.67    --   46.00  78.00  35.35   35
 12  \w     14.00  46.00   1.00    4.67    --   46.00  80.00-144.19   32
 13  \w     22.00  49.00   1.00    4.67    --   54.00  78.00 160.24   27
 14  \w     22.00  49.00   1.00    4.67    --   54.00  78.00   2.96   27
 15  \w     22.00  49.00   1.00    4.67    --   54.00  78.00  85.70   27
 16  \w     22.00  49.00   1.00    4.67    --   54.00  78.00 -95.82   27
 17  \w     31.00 135.00   1.00    4.67    --   62.00  75.00  87.27  104
 18  \w     31.00 136.00   1.00    4.67    --   62.00  77.00 -69.23  105
 19  \w     31.00 135.00   1.00    4.67    --   62.00  76.00  34.47  104
 20  \w     31.00 136.00   1.00    4.67    --   62.00  77.00 126.84  105
 21  \w     35.00 139.00   1.00    4.67    --   66.00  75.00-130.47  104
 22  \w     35.00 139.00   1.00    4.67    --   66.00  75.00 146.59  104
 23  \w     35.00 140.00   1.00    4.67    --   66.00  77.00-169.70  105
 24  \w     39.00 144.00   1.00    4.67    --   70.00  77.00   2.46  105
 25  \w     39.00 144.00   1.00    4.67    --   70.00  77.00 -14.40  105
 26  \w     39.00 143.00   1.00    4.67    --   70.00  74.00 -44.51  104
 27  \w     39.00 144.00   1.00    4.67    --   70.00  77.00-116.63  105
 28  \w     39.00 144.00   1.00    4.67    --   70.00  77.00  46.42  105
 29  \w     44.00 146.00   1.00    4.67    --   74.00  73.00  33.88  102
 30  \w     51.00 155.00   1.00   18.67    --   82.00  75.00  75.17  104
 31  \w     52.00 154.00   1.00   18.67    --   82.00  72.00 -12.60  102
 32  \w     54.00 153.00   1.00   18.67    --   82.00  65.00 138.12   99
 33  \w     56.00 152.00   1.00   18.67    --   82.00  54.00 -60.55   96
 34  \w     56.00 158.00   1.00   18.67    --   86.00  72.00 -60.43  102
 35  \w     57.00 157.00   1.00   18.67    --   86.00  69.00 110.98  100
 36  \w     58.00 156.00   1.00   18.67    --   86.00  61.00  64.50   98
 37  \w     55.00 159.00   1.00   18.67    --   86.00  74.00 171.20  104
 38  \w     59.00 163.00   1.00   18.67    --   90.00  74.00-123.38  104
 39  \w     60.00 162.00   1.00   18.67    --   90.00  72.00 151.91  102
 40  \w     59.00 163.00   1.00   18.67    --   90.00  74.00-141.66  104
 41  \w     74.00 172.00   1.00   18.67    --  102.00  64.00 165.96   98
 42  \w     78.00 178.00   1.00   18.67    --  109.86  77.00-180.00  100
 43  \w     78.00 178.00   1.00   18.67    --  109.86  77.00   0.00  100
 44  \w     78.00 178.00   1.00   18.67    --  109.86  77.00  90.00  100
 45  \w     82.00 178.00   1.00   18.67    --  109.86  61.00   0.00   96
 46  \w     78.00 178.00   1.00   18.67    --  109.86  77.00-150.00  100
 47  \w     78.00 178.00   1.00   18.67    --  109.86  77.00 -30.00  100
 48  \w     82.00 178.00   1.00   18.67    --  109.86  61.00 120.00   96
 49  \w     38.00 122.00   1.00   18.67    --  109.86-125.00-180.00   84
 50  \w     78.00 178.00   1.00   18.67    --  109.86  77.00 -90.00  100
 51  \w     78.00 178.00   1.00   18.67    --  109.86  77.00  60.00  100
 52  \w     78.00 178.00   1.00   18.67    --  109.86  77.00 -60.00  100
 53  \w     39.00 134.00   1.00   18.67    --  109.86 -45.00-120.00   95
 54  \w     29.00 109.00   1.00   18.67    --  109.86 -94.00-180.00   80
 55  \w     29.00 109.00   1.00   18.67    --  109.86 -94.00 -30.00   80
 56  \w     29.00 109.00   1.00   18.67    --  109.86 -94.00  60.00   80
 57  \w     29.00 109.00   1.00   18.67    --  109.86 -94.00-120.00   80
 58  \w     78.00 178.00   1.00   18.67    --  109.86  77.00-120.00  100
 59  \w     78.00 178.00   1.00   18.67    --  109.86  77.00  30.00  100
 60  \w     13.00  45.00   1.00    4.67    --   46.00  82.00  45.01   32
 61  \w     18.00  46.00   1.00    4.67    --   50.00  81.00 126.58   28
 62  \w     18.00  46.00   1.00    4.67    --   50.00  81.00-118.44   28
 63  \w     35.00 139.00   1.00    4.67    --   66.00  75.00 -33.85  104
;
_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      0.0144998000
_diffrn_orient_matrix_UB_12      0.0368542000
_diffrn_orient_matrix_UB_13      -0.0083284000
_diffrn_orient_matrix_UB_21      0.1129066000
_diffrn_orient_matrix_UB_22      -0.0051071000
_diffrn_orient_matrix_UB_23      -0.0366070000
_diffrn_orient_matrix_UB_31      -0.0388936000
_diffrn_orient_matrix_UB_32      -0.0010887000
_diffrn_orient_matrix_UB_33      -0.1107988000
_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  0.0639
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.003
_diffrn_reflns_Laue_measured_fraction_max 1.002
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            243961
_diffrn_reflns_point_group_measured_fraction_full 1.003
_diffrn_reflns_point_group_measured_fraction_max 1.002
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.349
_diffrn_reflns_theta_min         3.204
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.452
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.827
_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    1.596
_exptl_crystal_description       plate
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.846
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 0 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1408
_refine_ls_number_reflns         27491
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0596P)^2^+13.7534P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.971
_reflns_Friedel_fraction_full    1.003
_reflns_Friedel_fraction_max     1.002
_reflns_number_gt                26648
_reflns_number_total             27491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma53_15
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_original_cell_volume        6979.77(9)
_cod_database_code               7041627
_chemical_oxdiff_formula         'C33 H36 F Si Sn3'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_date_sample_data_collection 2016-06-10
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.810(8) 0.037(4) 0.142(6) 0.011(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C13(H13), C14(H14), C15(H15), C16(H16),
 C24(H24), C25(H25), C26(H26), C27(H27), C35(H35), C36(H36), C37(H37), C38(H38),
  C46(H46), C47(H47), C48(H48), C49(H49), C57(H57), C58(H58), C59(H59),
 C60(H60), C68(H68), C69(H69), C70(H70), C71(H71), C79(H79), C80(H80), C81(H81),
  C82(H82), C90(H90), C91(H91), C92(H92), C93(H93), C101(H101), C102(H102),
 C103(H103), C104(H104), C112(H112), C113(H113), C114(H114), C115(H115),
 C123(H123), C124(H124), C125(H125), C126(H126)
3.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C75(H75A,
 H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C86(H86A,H86B,H86C),
 C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C97(H97A,H97B,H97C), C98(H98A,H98B,
 H98C), C99(H99A,H99B,H99C), C108(H10D,H10E,H10F), C109(H10G,H10H,H10I),
 C110(H11D,H11E,H11F), C119(H11G,H11H,H11I), C120(H12A,H12B,H12C), C121(H12D,
 H12E,H12F), C130(H13A,H13B,H13C), C131(H13D,H13E,H13F), C132(H13G,H13H,H13I)
;
_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 2.472
_oxdiff_exptl_absorpt_empirical_full_min 0.610
_shelx_res_checksum              85427
_shelxl_version_number           2013-2