Tridentate Lewis acids with phenyl substituted 1,3,5-trisilacyclohexane backbones.
Weisheim, Eugen; Bücker, Lisa; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 45 (2015) 198–207; doi:10.1039/c5dt04208a

data_7037293
_publ_section_title
;
 Tridentate Lewis acids with phenyl substituted 1,3,5-trisilacyclohexane
 backbones.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              198
_journal_page_last               207
_journal_paper_doi               10.1039/c5dt04208a
_journal_volume                  45
_journal_year                    2015
_chemical_formula_moiety         'C27 H24 Si3'
_chemical_formula_sum            'C27 H24 Si3'
_chemical_formula_weight         432.73
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-09
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2015-08-20 deposited with the CCDC.
2015-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.103(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9247(5)
_cell_length_b                   10.2169(3)
_cell_length_c                   12.3529(4)
_cell_measurement_reflns_used    48650
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.5720
_cell_measurement_theta_min      4.6240
_cell_volume                     2403.46(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      100.0(1)
_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 0.9998
_diffrn_measurement_details
;
  1 omega  -64.00   30.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000  150.0000 94

  2 omega -110.00  -18.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000    0.0000 92

  3 omega -110.00  -18.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000  120.0000 92

  4 omega  -50.00   33.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   90.0000 83

  5 omega  -50.00   33.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -60.0000 83

  6 omega   13.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -180.0000 102

  7 omega    1.00   82.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  -99.0000    0.0000 81

  8 omega   23.00   97.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488 -125.0000 -120.0000 74

  9 omega   18.00  112.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000 -150.0000 94

 10 omega   13.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000    0.0000 102

 11 omega   13.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -90.0000 102

 12 omega   13.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   90.0000 102

 13 omega   85.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 93

 14 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 97

 15 omega   85.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 93

 16 omega   85.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 93

 17 omega   85.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 93

 18 omega   31.00  109.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   90.0000 78

 19 omega   82.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   71.0000 -168.2849 96

 20 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 97

 21 omega   85.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 93

 22 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 97

 23 omega   41.00   98.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 57

 24 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 97

 25 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 97

 26 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 97

 27 omega   85.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 93

 28 omega   31.00  109.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 78

 29 omega   85.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 93

 30 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 97

 31 omega   41.00  122.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -30.0000 81

 32 omega   85.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 93

 33 omega   41.00  122.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 81

 34 omega   85.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 93

 35 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 97

 36 omega   85.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 93

 37 omega   85.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 93

 38 omega   89.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -150.0000 89

 39 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 97

 40 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 97

 41 omega   89.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -120.0000 89

 42 omega   85.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 93

 43 omega   40.00  141.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -150.0000 101

 44 omega   41.00  122.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 81

 45 omega   31.00  109.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 78

 46 omega   84.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   65.0000  168.3487 94

 47 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   76.0000  143.6284 97

 48 omega -110.00   -8.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -77.0000  120.0000 102

 49 omega   18.00  112.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000 -180.0000 94

 50 omega   23.00  114.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000 -180.0000 91

 51 omega   13.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   30.0000 102

 52 omega   13.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -150.0000 102

 53 omega  -42.00  129.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488    0.0000 -120.0000 171

 54 omega   13.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -30.0000 102

 55 omega   23.00  114.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000    0.0000 91

 56 omega   18.00  112.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000    0.0000 94

 57 omega   10.00  120.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   19.0000 -180.0000 110

 58 omega  -42.00  129.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488    0.0000 -180.0000 171

 59 omega  -42.00  129.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488    0.0000 -150.0000 171

 60 omega   18.00  112.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000  -30.0000 94

 61 omega   23.00  114.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000  150.0000 91
;
_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      -0.0528419000
_diffrn_orient_matrix_UB_12      -0.0106321000
_diffrn_orient_matrix_UB_13      0.0688417000
_diffrn_orient_matrix_UB_21      -0.0562518000
_diffrn_orient_matrix_UB_22      0.0681567000
_diffrn_orient_matrix_UB_23      -0.0964303000
_diffrn_orient_matrix_UB_31      -0.0242382000
_diffrn_orient_matrix_UB_32      -0.1342641000
_diffrn_orient_matrix_UB_33      -0.0543350000
_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  0.0793
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            81599
_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         72.120
_diffrn_reflns_theta_min         4.644
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.889
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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    1.196
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.3006
_exptl_crystal_size_mid          0.1496
_exptl_crystal_size_min          0.0656
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         4735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0628P)^2^+1.1947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4521
_reflns_number_total             4735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04208a2.cif
_cod_data_source_block           all-cis-7
_cod_depositor_comments
'Adding full bibliography for 7037290--7037293.cif.'
_cod_original_cell_volume        2403.47(13)
_cod_database_code               7037293
_chemical_oxdiff_formula         'C27 H24 Si3'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_shelx_res_checksum              32880
_shelxl_version_number           2014-3