One-pot synthesis of halogen exchanged silsesquioxanes: octakis(3-bromopropyl)octasilsesquioxane and octakis(3-iodopropyl)octasilsesquioxane.
Ervithayasuporn, V.; Pornsamutsin, N.; Prangyoo, P.; Sammawutthichai, K.; Jaroentomeechai, T.; Phurat, C.; Teerawatananond, T.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 13747–13753; doi:10.1039/c3dt51373d

data_7023447
_publ_section_title
;
 One-pot synthesis of halogen exchanged silsesquioxanes:
 octakis(3-bromopropyl)octasilsesquioxane and
 octakis(3-iodopropyl)octasilsesquioxane.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13747
_journal_page_last               13753
_journal_paper_doi               10.1039/c3dt51373d
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C24 H48 I8 O12 Si8'
_chemical_formula_sum            'C24 H48 I8 O12 Si8'
_chemical_formula_weight         1768.54
_chemical_name_common            Octakis(3-iodopropyl)octasilsesquioxane
_chemical_name_systematic
;
Octakis(3-iodopropyl)octasilsesquioxane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-05-10 # Formatted by publCIF
;
_cell_angle_alpha                111.216(7)
_cell_angle_beta                 95.856(7)
_cell_angle_gamma                98.847(6)
_cell_formula_units_Z            1
_cell_length_a                   8.8808(15)
_cell_length_b                   12.262(2)
_cell_length_c                   12.529(2)
_cell_measurement_pressure       101.325
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.16
_cell_measurement_theta_min      2.36
_cell_volume                     1238.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'publCIF for Windows (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20149
_diffrn_reflns_theta_full        32.22
_diffrn_reflns_theta_max         32.22
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    5.251
_exptl_absorpt_correction_T_max  0.1098
_exptl_absorpt_correction_T_min  0.0392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.245
_refine_diff_density_min         -2.908
_refine_diff_density_rms         0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         8585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.820
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+7.1723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0823
_reflns_number_gt                8135
_reflns_number_total             8585
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt51373d.txt
_cod_data_source_block           T8-I
_cod_original_cell_volume        1238.1(4)
_cod_database_code               7023447