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_7037291
_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         'C21 H21 Cl3 Si3, 0.5 (C5 H12)'
_chemical_formula_sum            'C23.5 H27 Cl3 Si3'
_chemical_formula_weight         500.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-03-19
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.5592(2)
_cell_length_b                   7.97338(8)
_cell_length_c                   28.7174(3)
_cell_measurement_reflns_used    21348
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0390
_cell_measurement_theta_min      4.0880
_cell_volume                     4936.51(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'J. Appl. Cryst. (2007) 40, 786-790'
_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 0.9996
_diffrn_measured_fraction_theta_max 0.9973
_diffrn_measurement_details
;
  1 omega -112.00   -5.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000  -30.0000 107

  2 omega -110.00  -24.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000  -90.0000 86

  3 omega   14.00   61.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -60.0000 47

  4 omega   72.00  115.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  120.0000 43

  5 omega   70.00  107.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000  120.0000 37

  6 omega   16.00   76.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -150.0000 60

  7 omega   80.00  115.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -180.0000 35

  8 omega   58.00  106.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  178.0000   30.0000 48

  9 omega   88.00  115.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -60.0000 27

 10 omega   13.00   66.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   30.0000 53

 11 omega  -15.00   70.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  -77.0000 -150.0000 85

 12 omega    2.00   72.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  -99.0000   60.0000 70

 13 omega   14.00   51.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -180.0000 37

 14 omega   13.00   64.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  120.0000 51

 15 omega   87.00  113.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -150.0000 26

 16 omega   28.00   67.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000  120.0000 39

 17 omega   58.00  109.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  178.0000 -150.0000 51

 18 omega  113.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 62

 19 omega   86.00  112.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 26

 20 omega   53.00   93.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 40

 21 omega   50.00   89.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   90.0000 39

 22 omega   85.00  117.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 32

 23 omega   85.00  148.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 63

 24 omega   81.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 96

 25 omega  123.00  154.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 31

 26 omega   31.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 77

 27 omega   84.00  112.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   63.0000   42.1219 28

 28 omega   81.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 26

 29 omega   85.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   63.0000  -21.6687 25

 30 omega   85.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 26

 31 omega   41.00  121.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -30.0000 80

 32 omega   81.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 96

 33 omega   85.00  117.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 32

 34 omega   85.00  160.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 75

 35 omega   85.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 26

 36 omega   81.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 26

 37 omega   88.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   62.0000  -99.8401 27

 38 omega   81.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 26

 39 omega  113.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 64

 40 omega   86.00  112.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 26

 41 omega   89.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -90.0000 26

 42 omega   85.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 26

 43 omega   81.00  169.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 88

 44 omega   43.00  119.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 76

 45 omega   81.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 26

 46 omega  128.00  154.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 26

 47 omega   85.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 31

 48 omega   81.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 25

 49 omega  113.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 65

 50 omega   81.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 26

 51 omega  113.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 64

 52 omega   46.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 62

 53 omega   85.00  162.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 77

 54 omega   81.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 26

 55 omega   85.00  113.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 28

 56 omega   32.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 76

 57 omega   84.00  147.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   66.0000  -85.9326 63

 58 omega   87.00  161.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   57.0000  136.4041 74

 59 omega   82.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   71.0000  -61.8801 26
;
_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      0.0399271000
_diffrn_orient_matrix_UB_12      0.1566686000
_diffrn_orient_matrix_UB_13      -0.0092719000
_diffrn_orient_matrix_UB_21      0.0137197000
_diffrn_orient_matrix_UB_22      -0.0636748000
_diffrn_orient_matrix_UB_23      -0.0496049000
_diffrn_orient_matrix_UB_31      -0.0576637000
_diffrn_orient_matrix_UB_32      0.0932823000
_diffrn_orient_matrix_UB_33      -0.0182435000
_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  0.0424
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            45373
_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         76.28
_diffrn_reflns_theta_min         3.08
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.823
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.1172
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.0323
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0523P)^2^+3.5718P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2305
_reflns_number_total             2495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04208a2.cif
_cod_data_source_block           cis-trans-5
_cod_depositor_comments
'Adding full bibliography for 7037290--7037293.cif.'
_cod_original_cell_volume        4936.49(8)
_cod_original_formula_sum        'C23.50 H27 Cl3 Si3'
_cod_database_code               7037291
_chemical_oxdiff_formula         'C21 H21 Cl3 Si3'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12)
;
_shelxl_version_number           2013-2