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_7123264
_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         'C24 H30 Hg3 Si6, 2(C5 H5 N)'
_chemical_formula_sum            'C34 H40 Hg3 N2 Si6'
_chemical_formula_weight         1246.99
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-16
_audit_creation_method
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  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
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2015-08-12 deposited with the CCDC.    2019-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.5413(6)
_cell_length_b                   17.0430(9)
_cell_length_c                   30.480(12)
_cell_measurement_reflns_used    96193
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.3790
_cell_measurement_theta_min      1.8740
_cell_volume                     8073(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9976
_diffrn_measurement_details
;
  1 omega   -4.00   94.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640   77.0000 -120.0000 98

  2 omega    6.00   93.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640   57.0000    0.0000 87

  3 omega    6.00   93.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640   57.0000 -180.0000 87

  4 omega  -20.00   65.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640  -99.0000  -30.0000 85

  5 omega  -47.00   63.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640  -19.0000   90.0000 110

  6 omega  -43.00   43.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640  -57.0000   30.0000 86

  7 omega   -4.00   94.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640   77.0000   30.0000 98

  8 omega    6.00   93.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640   57.0000  120.0000 87

  9 omega  -20.00   65.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640  -99.0000  -90.0000 85

 10 omega   -8.00   73.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640 -113.0000  169.3386 81

 11 omega  -97.00  -35.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000 -178.0000   90.0000 62

 12 omega  -93.00    5.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -77.0000   60.0000 98

 13 omega    3.00   96.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640   38.0000  -30.0000 93

 14 omega  -13.00   97.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640   19.0000 -150.0000 110

 15 omega  -20.00   65.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640  -99.0000 -150.0000 85

 16 omega   -4.00   94.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640   77.0000  -90.0000 98

 17 omega    6.00   83.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640 -130.0000  103.7929 77

 18 omega  -20.00   65.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       24.9640  -99.0000   30.0000 85

 19 omega  -95.00   48.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -150.0000 143

 20 omega  -95.00   48.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -120.0000 143

 21 omega  -95.00   48.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  -90.0000 143

 22 omega  -95.00  -89.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  -60.0000 6
;
_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      -0.0016414000
_diffrn_orient_matrix_UB_12      0.0415501000
_diffrn_orient_matrix_UB_13      -0.0001313000
_diffrn_orient_matrix_UB_21      0.0184083000
_diffrn_orient_matrix_UB_22      0.0003935000
_diffrn_orient_matrix_UB_23      -0.0212771000
_diffrn_orient_matrix_UB_31      -0.0416763000
_diffrn_orient_matrix_UB_32      -0.0014532000
_diffrn_orient_matrix_UB_33      -0.0093924000
_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  0.0851
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            387982
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.142
_diffrn_reflns_theta_min         2.221
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.585
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    2.052
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.2992
_exptl_crystal_size_mid          0.1927
_exptl_crystal_size_min          0.1843
_refine_diff_density_max         1.914
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         11876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0082P)^2^+21.0659P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11143
_reflns_number_total             11876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02315a2.cif
_cod_data_source_block           euwe27
_cod_database_code               7123264
_chemical_oxdiff_formula         'C24 H30 Hg3 Si6'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelx_hkl_checksum              303
_shelx_res_checksum              41443
_shelxl_version_number           2013-2