Self-assembly of a Si-based cage by the formation of 24 equivalent covalent bonds.
Holmes, Jessica L.; Abrahams, Brendan F.; Ahveninen, Anna; Boughton, Berin A.; Hudson, Timothy A.; Robson, Richard; Thinagaran, Dinaiz; Chemical communications (Cambridge, England) 54 (2018) 11877–11880; doi:10.1039/c8cc06405a

data_7122419
_publ_section_title
;
 Self-assembly of a Si-based cage by the formation of 24 equivalent
 covalent bonds.
;
_journal_issue                   84
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11877
_journal_page_last               11880
_journal_paper_doi               10.1039/c8cc06405a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C120 H78 Cs4 O30 Si6, 1.8(Br)'
_chemical_formula_sum            'C152 H298 Br2 Cs4 N4 O94 Si6'
_chemical_formula_weight         4545.93
_space_group_crystal_system      cubic
_space_group_IT_number           216
_space_group_name_Hall           'F -4 2 3'
_space_group_name_H-M_alt        'F -4 3 m'
_symmetry_space_group_name_Hall  'F -4 2 3'
_symmetry_space_group_name_H-M   'F -4 3 m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-01-06
_audit_creation_method
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2018-08-05 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.7206(7)
_cell_length_b                   27.7206(7)
_cell_length_c                   27.7206(7)
_cell_measurement_reflns_used    1225
_cell_measurement_temperature    130.01(10)
_cell_measurement_theta_max      56.3330
_cell_measurement_theta_min      4.4830
_cell_volume                     21301.4(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.8266
_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    -64.00  -7.00   1.00    2.50    --  -41.74 125.00 150.00   57
  2  \w     85.00 177.00   1.00   15.00    --  112.00  30.00 120.00   92
  3  \w     47.00  83.00   1.00   15.00    --  112.00 -30.00-120.00   36
;
_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      0.0126962000
_diffrn_orient_matrix_UB_12      -0.0488957000
_diffrn_orient_matrix_UB_13      -0.0233840000
_diffrn_orient_matrix_UB_21      0.0340060000
_diffrn_orient_matrix_UB_22      0.0258875000
_diffrn_orient_matrix_UB_23      -0.0356165000
_diffrn_orient_matrix_UB_31      0.0420345000
_diffrn_orient_matrix_UB_32      -0.0061199000
_diffrn_orient_matrix_UB_33      0.0356011000
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5561
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.776
_diffrn_reflns_theta_min         4.512
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       tetrahedron
_exptl_crystal_F_000             9456
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.092
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.293
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1670
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.298
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.1023
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2762
_refine_ls_wR_factor_ref         0.2864
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1508
_reflns_number_total             1670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06405a2.cif
_cod_data_source_block           jlh_sitet_csbr_soak_sx
_cod_depositor_comments
'Adding full bibliography for 7122418--7122419.cif.'
_cod_original_cell_volume        21301.4(16)
_cod_database_code               7122419
_chemical_oxdiff_usercomment
'light yellow chunk. crystal of si tet soaked in aq CsBr 30 mg. Dec 17 2017 '
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.91(2) 0.09(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C5-C6 = C6-C7 = C7-C8
 1.39 with sigma of 0.01
 C5-C8
 2.78 with sigma of 0.01
 C8-H8
 0.93 with sigma of 0.01
 C6-C7 \\sim C7-C8
 with sigma of 0.02
4. Restrained planarity
 C5, C6, C8, C7
 with sigma of 0.1
 C5, C6, C7, C8
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
6. Others
 Fixed Sof: Br1(0.03333) C6(0.5) H6(0.5) O5(0.25) C7(0.5) H7(0.5) Br2(0.00833)
7.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7)
;
_shelx_res_checksum              35577
_shelx_fab_checksum              62323
_shelx_shelxl_version_number     2018/1
_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 1.445
_oxdiff_exptl_absorpt_empirical_full_min 0.782