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_7123263
_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         'C78 H90 Li6 O6 Si6'
_chemical_formula_sum            'C78 H90 Li6 O6 Si6'
_chemical_formula_weight         1333.67
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-01-18
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.1176(2)
_cell_length_b                   12.1176(2)
_cell_length_c                   44.8866(8)
_cell_measurement_reflns_used    33536
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.2260
_cell_measurement_theta_min      4.3050
_cell_volume                     5707.96(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.30a (Agilent, 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      200.00(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 0.9985
_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    -66.00  35.00   1.00    4.86    --  -38.50  83.00-178.00  101
  2  \w     -5.00  73.00   1.00    4.86    --   43.45 -83.00  61.00   78
  3  \w     37.00 142.00   1.00   15.00    --  111.00 -83.00  61.00  105
  4  \w    113.00 138.00   1.00   15.00    --  111.00  83.00-178.00   25
  5  \w   -107.00  -8.00   1.00    4.86    --  -38.50 -19.00 150.00   99
  6  \w    -64.00  28.00   1.00    4.86    --  -38.50  57.00 -30.00   92
  7  \w     13.00 114.00   1.00    4.86    --   43.45  77.00 -60.00  101
  8  \w     18.00  73.00   1.00    4.86    --   43.45  77.00-180.00   55
  9  \w     49.00  82.00   1.00    4.86    --   43.45-125.00 -30.00   33
 10  \w     13.00 113.00   1.00    4.86    --   43.45  77.00  60.00  100
 11  \w     14.00  68.00   1.00    4.86    --   43.45  77.00-120.00   54
 12  \w     19.00  76.00   1.00    4.86    --   43.45  57.00   0.00   57
 13  \w     76.00 102.00   1.00    4.86    --   43.45  77.00-180.00   26
 14  \w     15.00  87.00   1.00    4.86    --   43.45  77.00   0.00   72
 15  \w     24.00 113.00   1.00    4.86    --   43.45  38.00 -90.00   89
 16  \w     18.00  83.00   1.00    4.86    --   43.45  77.00 120.00   65
 17  \w     81.00 178.00   1.00   15.00    --  111.00  77.00  60.00   97
 18  \w     85.00 111.00   1.00   15.00    --  111.00  61.00-120.00   26
 19  \w     81.00 107.00   1.00   15.00    --  111.00  77.00   0.00   26
 20  \w     83.00 108.00   1.00   15.00    --  111.00  68.00 121.28   25
 21  \w     53.00 137.00   1.00   15.00    --  111.00 -61.00 -90.00   84
 22  \w     85.00 110.00   1.00   15.00    --  111.00  61.00  90.00   25
 23  \w     82.00 108.00   1.00   15.00    --  111.00  72.00 -97.74   26
 24  \w     85.00 112.00   1.00   15.00    --  111.00  61.00  60.00   27
 25  \w     83.00 108.00   1.00   15.00    --  111.00  68.00  -7.92   25
 26  \w     81.00 174.00   1.00   15.00    --  111.00  77.00  90.00   93
 27  \w     81.00 106.00   1.00   15.00    --  111.00  77.00-167.89   25
 28  \w     81.00 177.00   1.00   15.00    --  111.00  77.00 120.00   96
 29  \w     81.00 112.00   1.00   15.00    --  111.00  77.00 -90.00   31
 30  \w    119.00 163.00   1.00   15.00    --  111.00  77.00 -90.00   44
 31  \w     85.00 177.00   1.00   15.00    --  111.00  61.00 -30.00   92
 32  \w     81.00 107.00   1.00   15.00    --  111.00  77.00  30.00   26
 33  \w     85.00 111.00   1.00   15.00    --  111.00  61.00 120.00   26
 34  \w     81.00 106.00   1.00   15.00    --  111.00  77.00 -30.00   25
 35  \w     84.00 110.00   1.00   15.00    --  111.00  63.00-109.00   26
 36  \w     81.00 176.00   1.00   15.00    --  111.00  77.00 -60.00   95
 37  \w     82.00 108.00   1.00   15.00    --  111.00  73.00 143.47   26
 38  \w     85.00 157.00   1.00   15.00    --  111.00  59.00 -58.91   72
 39  \w     81.00 107.00   1.00   15.00    --  111.00  77.00-180.00   26
 40  \w     84.00 122.00   1.00   15.00    --  111.00-125.00  60.00   38
 41  \w     49.00 122.00   1.00   15.00    --  111.00-125.00-120.00   73
 42  \w     82.00 108.00   1.00   15.00    --  111.00  73.00 -66.00   26
 43  \w     83.00 108.00   1.00   15.00    --  111.00  69.00 -30.71   25
 44  \w     82.00 178.00   1.00   15.00    --  111.00  77.00-120.00   96
 45  \w     85.00 177.00   1.00   15.00    --  111.00  61.00-180.00   92
 46  \w     85.00 110.00   1.00   15.00    --  111.00  61.00 -90.00   25
 47  \w     85.00 111.00   1.00   15.00    --  111.00  60.00  72.30   26
 48  \w     85.00 112.00   1.00   15.00    --  111.00  61.00 150.00   27
 49  \w     81.00 166.00   1.00   15.00    --  111.00  77.00 150.00   85
 50  \w    113.00 178.00   1.00   15.00    --  111.00  77.00-150.00   65
 51  \w    127.00 166.00   1.00   15.00    --  111.00  58.00  14.84   39
 52  \w     86.00 121.00   1.00   15.00    --  111.00  58.00  14.84   35
 53  \w     41.00 121.00   1.00   15.00    --  111.00-125.00 -90.00   80
 54  \w     88.00 113.00   1.00   15.00    --  111.00  46.00-125.77   25
 55  \w     84.00 137.00   1.00   15.00    --  111.00 -61.00  30.00   53
 56  \w     88.00 160.00   1.00   15.00    --  111.00  48.00  43.54   72
 57  \w     81.00 106.00   1.00   15.00    --  111.00  77.00-150.00   25
 58  \w     86.00 111.00   1.00   15.00    --  111.00  58.00  38.49   25
 59  \w     31.00 108.00   1.00   15.00    --  111.00 -94.00 -90.00   77
;
_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      0.1125744000
_diffrn_orient_matrix_UB_12      -0.0013333000
_diffrn_orient_matrix_UB_13      -0.0156193000
_diffrn_orient_matrix_UB_21      0.0077930000
_diffrn_orient_matrix_UB_22      -0.0802060000
_diffrn_orient_matrix_UB_23      0.0256640000
_diffrn_orient_matrix_UB_31      -0.0939094000
_diffrn_orient_matrix_UB_32      -0.1228988000
_diffrn_orient_matrix_UB_33      -0.0165922000
_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  0.0328
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            63931
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.957
_diffrn_reflns_theta_min         2.953
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.406
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.30a (Agilent, 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    1.164
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4146
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0601P)^2^+1.9660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3872
_reflns_number_total             4146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02315a2.cif
_cod_data_source_block           compound2bx6THF
_cod_original_cell_volume        5708.0(2)
_cod_database_code               7123263
_chemical_oxdiff_formula         'C78 H90 Li6 O6 Si6'
_chemical_oxdiff_usercomment     ' '
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_date_sample_data_collection 2015-10-20
_olex2_date_sample_submission    1444600800
_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 1.218
_oxdiff_exptl_absorpt_empirical_full_min 0.865
_shelx_hkl_checksum              12734
_shelx_res_checksum              31555
_shelxl_version_number           2014-3