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_7123261
_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         'C48 H78 Li6 O6 Si6'
_chemical_formula_sum            'C48 H78 Li6 O6 Si6'
_chemical_formula_weight         961.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
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2015-08-12 deposited with the CCDC.    2019-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                108.601(8)
_cell_angle_beta                 104.450(7)
_cell_angle_gamma                104.858(8)
_cell_formula_units_Z            1
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_cell_length_b                   11.8325(13)
_cell_length_c                   13.6055(10)
_cell_measurement_reflns_used    9173
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.8480
_cell_measurement_theta_min      1.9510
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics
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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
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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 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9989
_diffrn_measurement_details
;
  1 omega  -15.00   65.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7145  -99.0000  -30.0000 80

  2 omega  -20.00    6.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7145  -99.0000   30.0000 26

  3 omega  -19.00   65.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7145  -99.0000   60.0000 84

  4 omega   -4.00   87.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7145   19.0000  150.0000 91

  5 omega  -39.00   53.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7145  -77.0000 -150.0000 92

  6 omega    6.00   93.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7145   57.0000 -180.0000 87

  7 omega   -4.00   89.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7145   77.0000 -120.0000 93

  8 omega   -1.00   59.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7145   77.0000   60.0000 60

  9 omega    0.00   94.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7145   77.0000  -30.0000 94

 10 omega  -44.00   53.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7145  -77.0000  120.0000 97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0035808000
_diffrn_orient_matrix_UB_12      0.0192668000
_diffrn_orient_matrix_UB_13      0.0539327000
_diffrn_orient_matrix_UB_21      0.0378133000
_diffrn_orient_matrix_UB_22      0.0647844000
_diffrn_orient_matrix_UB_23      0.0115504000
_diffrn_orient_matrix_UB_31      -0.0666212000
_diffrn_orient_matrix_UB_32      0.0071323000
_diffrn_orient_matrix_UB_33      -0.0208775000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27424
_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         29.999
_diffrn_reflns_theta_min         1.951
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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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    1.131
_exptl_crystal_description       block
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.1605
_exptl_crystal_size_mid          0.1184
_exptl_crystal_size_min          0.0755
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         8221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0406P)^2^+0.8912P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6372
_reflns_number_total             8221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02315a2.cif
_cod_data_source_block           euwe25
_cod_original_cell_volume        1410.9(2)
_cod_database_code               7123261
_chemical_oxdiff_formula         'C24 H39 Li3 O3 Si3'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelx_hkl_checksum              13922
_shelx_res_checksum              70655
_shelxl_version_number           2013-2