#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/34/7023447.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7023447
loop_
_publ_author_name
'Ervithayasuporn, V.'
'Pornsamutsin, N.'
'Prangyoo, P.'
'Sammawutthichai, K.'
'Jaroentomeechai, T.'
'Phurat, C.'
'Teerawatananond, T.'
_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/[σ²(Fo²)+(0.0484P)²+7.1723P] where P=(Fo²+2Fc²)/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     >2σ(I)
_cod_data_source_file            c3dt51373d.txt
_cod_data_source_block           T8-I
_cod_original_cell_volume        1238.1(4)
_cod_database_code               7023447
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.3264(3) 0.2904(2) 0.4098(2) 0.0107(4) Uani 1 1 d U
H1A H 0.4068 0.3623 0.4403 0.013 Uiso 1 1 calc R
H1B H 0.3114 0.2620 0.3257 0.013 Uiso 1 1 calc R
C2 C 0.1764(3) 0.3236(2) 0.4492(2) 0.0127(4) Uani 1 1 d U
H2A H 0.1059 0.2515 0.4418 0.015 Uiso 1 1 calc R
H2B H 0.1993 0.3761 0.5307 0.015 Uiso 1 1 calc R
C3 C 0.0965(3) 0.3847(2) 0.3812(3) 0.0197(5) Uani 1 1 d U
H3A H -0.0018 0.3962 0.4060 0.024 Uiso 1 1 calc R
H3B H 0.0757 0.3334 0.2993 0.024 Uiso 1 1 calc R
C4 C 0.7959(3) 0.1103(2) 0.2684(2) 0.0103(4) Uani 1 1 d U
H4A H 0.8067 0.1956 0.2882 0.012 Uiso 1 1 calc R
H4B H 0.8985 0.0949 0.2825 0.012 Uiso 1 1 calc R
C5 C 0.7292(3) 0.0447(2) 0.1393(2) 0.0138(4) Uani 1 1 d U
H5A H 0.7224 -0.0405 0.1177 0.017 Uiso 1 1 calc R
H5B H 0.6256 0.0581 0.1244 0.017 Uiso 1 1 calc R
C6 C 0.8298(3) 0.0885(2) 0.0670(2) 0.0137(4) Uani 1 1 d U
H6A H 0.9350 0.0802 0.0862 0.016 Uiso 1 1 calc R
H6B H 0.8310 0.1726 0.0855 0.016 Uiso 1 1 calc R
C10 C 0.5337(3) 0.3143(2) 0.8379(2) 0.0101(4) Uani 1 1 d U
H10A H 0.6074 0.3813 0.8376 0.012 Uiso 1 1 calc R
H10B H 0.4345 0.3379 0.8431 0.012 Uiso 1 1 calc R
C11 C 0.5849(3) 0.2913(2) 0.9475(2) 0.0118(4) Uani 1 1 d U
H11A H 0.5135 0.2239 0.9494 0.014 Uiso 1 1 calc R
H11B H 0.6870 0.2724 0.9467 0.014 Uiso 1 1 calc R
C12 C 0.5879(3) 0.4018(2) 1.0533(2) 0.0135(4) Uani 1 1 d U
H12A H 0.4863 0.4215 1.0507 0.016 Uiso 1 1 calc R
H12B H 0.6605 0.4679 1.0502 0.016 Uiso 1 1 calc R
C13 C 0.0001(3) -0.1341(2) 0.3138(2) 0.0108(4) Uani 1 1 d U
H13A H -0.0653 -0.0906 0.3637 0.013 Uiso 1 1 calc R
H13B H -0.0082 -0.1156 0.2447 0.013 Uiso 1 1 calc R
C14 C -0.0622(3) -0.2678(2) 0.2778(2) 0.0141(4) Uani 1 1 d U
H14A H -0.0311 -0.2902 0.3421 0.017 Uiso 1 1 calc R
H14B H -0.1743 -0.2826 0.2633 0.017 Uiso 1 1 calc R
C15 C -0.0091(4) -0.3469(3) 0.1716(3) 0.0208(5) Uani 1 1 d U
H15A H -0.0403 -0.4296 0.1625 0.025 Uiso 1 1 calc R
H15B H 0.1029 -0.3278 0.1828 0.025 Uiso 1 1 calc R
I1 I 0.23294(2) 0.554892(17) 0.40420(2) 0.02714(6) Uani 1 1 d U
I2 I 0.74781(2) -0.009853(18) -0.115314(14) 0.01837(5) Uani 1 1 d U
I4 I 0.65147(3) 0.384728(18) 1.216508(15) 0.02227(5) Uani 1 1 d U
I5 I -0.10284(3) -0.32735(2) 0.013998(17) 0.02750(6) Uani 1 1 d U
O1 O 0.5372(2) 0.13738(17) 0.38735(17) 0.0123(3) Uani 1 1 d U
O2 O 0.2123(2) -0.09646(17) 0.51276(16) 0.0110(3) Uani 1 1 d U
O4 O 0.4541(2) 0.22500(16) 0.59266(15) 0.0108(3) Uani 1 1 d U
O5 O 0.3170(2) -0.15350(16) 0.31592(16) 0.0103(3) Uani 1 1 d U
O9 O 0.2557(2) 0.06115(15) 0.41592(16) 0.0110(3) Uani 1 1 d U
O10 O 0.6063(2) -0.07441(15) 0.30490(16) 0.0102(3) Uani 1 1 d U
Si1 Si 0.39548(8) 0.17644(6) 0.45356(6) 0.00687(11) Uani 1 1 d U
Si2 Si 0.67805(8) 0.06699(6) 0.36452(6) 0.00672(11) Uani 1 1 d U
Si4 Si 0.51567(8) 0.18795(5) 0.69871(5) 0.00621(11) Uani 1 1 d U
Si5 Si 0.20161(7) -0.07907(6) 0.39007(6) 0.00642(11) Uani 1 1 d U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 C1 Si1 115.91(17) . .
C3 C2 C1 113.9(2) . .
C2 C3 I1 112.36(18) . .
C5 C4 Si2 113.93(17) . .
C6 C5 C4 110.5(2) . .
C5 C6 I2 111.51(17) . .
C11 C10 Si4 115.85(16) . .
C12 C11 C10 108.9(2) . .
C11 C12 I4 114.35(17) . .
C14 C13 Si5 115.40(17) . .
C15 C14 C13 114.8(2) . .
C14 C15 I5 112.7(2) . .
Si1 O1 Si2 152.42(13) . .
Si2 O2 Si5 145.07(13) 2_656 .
Si1 O4 Si4 144.67(12) . .
Si4 O5 Si5 152.17(13) 2_656 .
Si5 O9 Si1 148.38(13) . .
Si4 O10 Si2 148.91(13) 2_656 .
O1 Si1 O9 109.24(10) . .
O1 Si1 O4 108.94(11) . .
O9 Si1 O4 108.76(10) . .
O1 Si1 C1 108.84(11) . .
O9 Si1 C1 108.88(11) . .
O4 Si1 C1 112.14(11) . .
O10 Si2 O1 108.47(10) . .
O10 Si2 O2 109.32(10) . 2_656
O1 Si2 O2 109.52(10) . 2_656
O10 Si2 C4 109.07(10) . .
O1 Si2 C4 111.62(11) . .
O2 Si2 C4 108.82(11) 2_656 .
O10 Si4 O5 109.71(10) 2_656 2_656
O10 Si4 O4 108.58(10) 2_656 .
O5 Si4 O4 109.63(10) 2_656 .
O10 Si4 C10 110.13(11) 2_656 .
O5 Si4 C10 109.10(11) 2_656 .
O4 Si4 C10 109.68(10) . .
O9 Si5 O5 109.81(10) . .
O9 Si5 O2 108.78(10) . .
O5 Si5 O2 107.88(10) . .
O9 Si5 C13 110.22(11) . .
O5 Si5 C13 111.45(11) . .
O2 Si5 C13 108.63(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.529(4) .
C1 Si1 1.838(2) .
C2 C3 1.514(4) .
C3 I1 2.149(3) .
C4 C5 1.526(3) .
C4 Si2 1.838(2) .
C5 C6 1.509(4) .
C6 I2 2.145(3) .
C10 C11 1.537(3) .
C10 Si4 1.838(2) .
C11 C12 1.509(3) .
C12 I4 2.157(3) .
C13 C14 1.527(4) .
C13 Si5 1.840(3) .
C14 C15 1.506(4) .
C15 I5 2.172(3) .
O1 Si1 1.616(2) .
O1 Si2 1.618(2) .
O2 Si2 1.6208(19) 2_656
O2 Si5 1.6220(19) .
O4 Si1 1.6222(19) .
O4 Si4 1.6233(19) .
O5 Si4 1.6163(19) 2_656
O5 Si5 1.6170(19) .
O9 Si5 1.6134(19) .
O9 Si1 1.6185(19) .
O10 Si4 1.6108(19) 2_656
O10 Si2 1.6110(19) .
Si2 O2 1.621(2) 2_656
Si4 O10 1.6108(19) 2_656
Si4 O5 1.6163(19) 2_656
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 15204052
