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_7037290
_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         'C24 H30 O3 Si3'
_chemical_formula_sum            'C24 H30 O3 Si3'
_chemical_formula_weight         450.75
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-11-12
_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                 91.6490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.64716(11)
_cell_length_b                   21.6495(2)
_cell_length_c                   11.66228(13)
_cell_measurement_reflns_used    51500
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      32.0190
_cell_measurement_theta_min      2.9330
_cell_volume                     2434.73(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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_temperature      99.99(10)
_diffrn_detector_area_resol_mean 8.0951
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9613
_diffrn_measurement_details
;
  1 omega  -42.00   81.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421    0.0000  150.0000 123

  2 omega    3.00   96.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421   38.0000    0.0000 93

  3 omega  -20.00   66.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000  150.0000 86

  4 omega  -16.00   66.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000  -30.0000 82

  5 omega   -4.00   86.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000  120.0000 90

  6 omega   -4.00   65.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000 -120.0000 69

  7 omega   63.00   99.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421  178.0000  -30.0000 36

  8 omega   60.00  100.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421 -178.0000  150.0000 40

  9 omega   -4.00   79.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000    0.0000 83

 10 omega  -32.00   92.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421    0.0000  -60.0000 124

 11 omega  -79.00   -3.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  127.0000  128.0000 76

 12 omega   35.00   99.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421  178.0000   30.0000 64

 13 omega   -4.00   94.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000    0.0000 98

 14 omega    7.00   93.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000  -60.0000 86

 15 omega    7.00   93.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000 -180.0000 86

 16 omega    7.00   93.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000  120.0000 86

 17 omega  -20.00   66.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000  120.0000 86

 18 omega  -43.00   44.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -57.0000   30.0000 87

 19 omega  -97.00  -35.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -      -23.5000 -178.0000   60.0000 62

 20 omega   34.00  100.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421 -178.0000  -60.0000 66

 21 omega  -20.00   66.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000  -30.0000 86

 22 omega    3.00   96.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421   38.0000   60.0000 93

 23 omega   -4.00   94.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000 -180.0000 98

 24 omega    3.00   13.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       25.0421   38.0000  -90.0000 10
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0402072000
_diffrn_orient_matrix_UB_12      -0.0006135000
_diffrn_orient_matrix_UB_13      0.0499540000
_diffrn_orient_matrix_UB_21      -0.0042511000
_diffrn_orient_matrix_UB_22      0.0327025000
_diffrn_orient_matrix_UB_23      -0.0010710000
_diffrn_orient_matrix_UB_31      -0.0614447000
_diffrn_orient_matrix_UB_32      -0.0018888000
_diffrn_orient_matrix_UB_33      -0.0347238000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            112581
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.080
_diffrn_reflns_theta_min         2.568
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.3731
_exptl_crystal_size_mid          0.3391
_exptl_crystal_size_min          0.0688
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         7153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0319P)^2^+1.4707P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6714
_reflns_number_total             7153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04208a2.cif
_cod_data_source_block           all-cis-4
_cod_depositor_comments
'Adding full bibliography for 7037290--7037293.cif.'
_cod_original_cell_volume        2434.74(5)
_cod_database_code               7037290
_chemical_oxdiff_formula         'C24 H30 O3 Si3'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_shelx_res_checksum              83957
_shelxl_version_number           2013-2