Trifunctional organometallic frameworks and cages based on all-cis-1,3,5-triethynyl-1,3,5-trisilacyclohexanes
Weisheim, Eugen; Weigel, Simon; Neumann, Beate; Stammler, Georg; Mitzel, Norbert Werner; Chemical Communications  (2019) –; doi:10.1039/C9CC02315A

data_7123262
_publ_section_title
;
 Trifunctional organometallic frameworks and cages based on
 all-cis-1,3,5-triethynyl-1,3,5-trisilacyclohexanes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02315A
_journal_year                    2019
_chemical_formula_moiety         'C36 H48 Si6'
_chemical_formula_sum            'C36 H48 Si6'
_chemical_formula_weight         649.28
_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             2016-01-05
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2019-03-08 deposited with the CCDC.    2019-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.9949(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.69042(8)
_cell_length_b                   32.0784(2)
_cell_length_c                   12.72592(10)
_cell_measurement_reflns_used    66184
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0940
_cell_measurement_theta_min      3.8000
_cell_volume                     3986.98(6)
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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   -109.00 -17.00   1.00    2.50    --  -38.50 -40.00 -67.00   92
  2  \w   -122.00 -35.00   1.00    2.50    --  -38.50-178.00 -30.00   87
  3  \w    -64.00  30.00   1.00    2.50    --  -38.50  57.00   0.00   94
  4  \w     57.00 127.00   1.00    2.50    --   43.45 178.00-120.00   70
  5  \w     22.00 114.00   1.00    2.50    --   43.45  40.00  85.00   92
  6  \w     57.00 127.00   1.00    2.50    --   43.45 178.00 -30.00   70
  7  \w     13.00 115.00   1.00    2.50    --   43.45  77.00 150.00  102
  8  \w     13.00 115.00   1.00    2.50    --   43.45  77.00  90.00  102
  9  \w     13.00 115.00   1.00    2.50    --   43.45  77.00  30.00  102
 10  \w     13.00 115.00   1.00    2.50    --   43.45  77.00 -90.00  102
 11  \w     13.00 115.00   1.00    2.50    --   43.45  77.00 -30.00  102
 12  \w     12.00  46.00   1.00    2.50    --   43.45  81.00 178.37   34
 13  \w     18.00 112.00   1.00    2.50    --   43.45  57.00 -90.00   94
 14  \w     18.00 112.00   1.00    2.50    --   43.45  57.00-150.00   94
 15  \w     82.00 178.00   1.00   10.00    --  111.00  74.00-135.24   96
 16  \w     81.00 178.00   1.00   10.00    --  111.00  76.00 -88.22   97
 17  \w     85.00 178.00   1.00   10.00    --  111.00  62.00   7.19   93
 18  \w     85.00 178.00   1.00   10.00    --  111.00  61.00  30.00   93
 19  \w     82.00 178.00   1.00   10.00    --  111.00  71.00-115.75   96
 20  \w     31.00 109.00   1.00   10.00    --  111.00 -94.00 150.00   78
 21  \w     81.00 162.00   1.00   10.00    --  111.00  77.00-180.00   81
 22  \w     85.00 177.00   1.00   10.00    --  111.00  61.00  60.00   92
 23  \w     43.00 137.00   1.00   10.00    --  111.00 -61.00 -90.00   94
 24  \w     53.00 122.00   1.00   10.00    --  111.00-125.00 -90.00   69
 25  \w     85.00 165.00   1.00   10.00    --  111.00  61.00 150.00   80
 26  \w     86.00 113.00   1.00   10.00    --  111.00  61.00 -51.62   27
 27  \w     83.00 109.00   1.00   10.00    --  111.00  70.00  85.07   26
 28  \w    143.00 169.00   1.00   10.00    --  111.00  77.00 120.00   26
 29  \w     31.00  98.00   1.00   10.00    --  111.00 -94.00 -90.00   67
 30  \w     85.00 111.00   1.00   10.00    --  111.00  61.00 130.44   26
 31  \w     37.00 105.00   1.00   10.00    --  111.00 -94.00  90.00   68
 32  \w     81.00 114.00   1.00   10.00    --  111.00  77.00 150.00   33
 33  \w     81.00 107.00   1.00   10.00    --  111.00  77.00   0.00   26
 34  \w     48.00  75.00   1.00   10.00    --  111.00 -94.00-150.00   27
 35  \w     82.00 157.00   1.00   10.00    --  111.00  71.00 -88.13   75
 36  \w     82.00 109.00   1.00   10.00    --  111.00  72.00-158.11   27
 37  \w     85.00 165.00   1.00   10.00    --  111.00  61.00  90.00   80
 38  \w     81.00 107.00   1.00   10.00    --  111.00  77.00 120.00   26
 39  \w     81.00 134.00   1.00   10.00    --  111.00  77.00-150.00   53
 40  \w     85.00 111.00   1.00   10.00    --  111.00  61.00 -60.00   26
 41  \w     81.00 152.00   1.00   10.00    --  111.00  77.00  30.00   71
 42  \w     85.00 111.00   1.00   10.00    --  111.00  61.00 -30.00   26
 43  \w     81.00 108.00   1.00   10.00    --  111.00  77.00  60.00   27
 44  \w     85.00 132.00   1.00   10.00    --  111.00  61.00-150.00   47
 45  \w     85.00 114.00   1.00   10.00    --  111.00  61.00   0.00   29
 46  \w     85.00 110.00   1.00   10.00    --  111.00  61.00 -90.00   25
 47  \w     81.00 177.00   1.00   10.00    --  111.00  77.00 -60.00   96
 48  \w     83.00 114.00   1.00   10.00    --  111.00  68.00  65.22   31
 49  \w     85.00 169.00   1.00   10.00    --  111.00  61.00-180.00   84
 50  \w    118.00 177.00   1.00   10.00    --  111.00  77.00 -30.00   59
 51  \w     83.00 109.00   1.00   10.00    --  111.00 -94.00 -60.00   26
 52  \w     41.00 122.00   1.00   10.00    --  111.00-125.00  90.00   81
 53  \w     81.00 115.00   1.00   10.00    --  111.00  77.00 -30.00   34
 54  \w     82.00 108.00   1.00   10.00    --  111.00  72.00 -38.21   26
 55  \w     84.00 110.00   1.00   10.00    --  111.00  64.00 103.09   26
 56  \w     82.00 177.00   1.00   10.00    --  111.00  72.00 103.45   95
;
_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      -0.0892916000
_diffrn_orient_matrix_UB_12      -0.0239906000
_diffrn_orient_matrix_UB_13      -0.1099126000
_diffrn_orient_matrix_UB_21      -0.1143668000
_diffrn_orient_matrix_UB_22      -0.0037161000
_diffrn_orient_matrix_UB_23      0.0437640000
_diffrn_orient_matrix_UB_31      -0.0618532000
_diffrn_orient_matrix_UB_32      0.0414369000
_diffrn_orient_matrix_UB_33      -0.0597158000
_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  0.0212
_diffrn_reflns_av_unetI/netI     0.0078
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            90276
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.227
_diffrn_reflns_theta_min         4.044
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.116
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.788
_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    1.082
_exptl_crystal_description       plank
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.00016(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+1.6290P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8240
_reflns_number_total             8336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02315a2.cif
_cod_data_source_block           compound3b
_cod_database_code               7123262
_chemical_oxdiff_formula         'C36 H48 Si6'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_date_sample_data_collection 2016-01-04
_olex2_refinement_description
;
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.094
_oxdiff_exptl_absorpt_empirical_full_min 0.904
_shelx_hkl_checksum              71708
_shelx_res_checksum              78078
_shelxl_version_number           2013-2