#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:36:23 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179538 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/07/4500799.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_4500799
loop_
_publ_author_name
'Roll, Mark F.'
'Kampf, Jeffrey W.'
'Laine, Richard M.'
_publ_section_title
;
 Halogen Bonding Motifs in Polyhedral Phenylsilsesquioxanes: Effects of
 Systematic Variations in Geometry or Substitution
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4360
_journal_paper_doi               10.1021/cg200312g
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         'C48 H24 Br16 O12 Si8, C S2'
_chemical_formula_sum            'C49 H24 Br16 O12 S2 Si8'
_chemical_formula_weight         2372.08
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                97.592(1)
_cell_angle_beta                 109.075(1)
_cell_angle_gamma                116.231(1)
_cell_formula_units_Z            1
_cell_length_a                   12.7172(9)
_cell_length_b                   12.7392(9)
_cell_length_c                   13.0890(9)
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      29.65
_cell_measurement_theta_min      2.40
_cell_volume                     1699.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            66787
_diffrn_reflns_theta_full        29.65
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    9.681
_exptl_absorpt_correction_T_max  0.3812
_exptl_absorpt_correction_T_min  0.1677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2008/1) Bruker AXS area
  detector absorption and other corrections, University of
  Gottingen, Germany 2008.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.429
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         9554
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0369P)²+3.7165P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                8581
_reflns_number_total             9554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200312g_si_002.cif
_cod_data_source_block           brops
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4500799
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.83252(3) 0.52348(2) 0.39819(2) 0.02114(6) Uani 1 1 d . . .
Br2 Br 0.49649(3) -0.07972(3) 0.17062(4) 0.03210(8) Uani 1 1 d . . .
Br3 Br 0.20389(3) 0.07790(3) 0.05276(2) 0.02495(6) Uani 1 1 d . . .
Br4 Br -0.00150(3) -0.15385(3) -0.49774(2) 0.02608(7) Uani 1 1 d . . .
Br5 Br -0.01836(3) 0.23088(3) -0.24463(3) 0.03688(8) Uani 1 1 d . . .
Br6 Br -0.00570(3) 0.45651(3) 0.23953(3) 0.03139(7) Uani 1 1 d . . .
Br7 Br 0.29125(3) 0.37493(3) 0.27315(3) 0.03014(7) Uani 1 1 d . . .
Br8 Br 0.74262(4) 0.92074(3) 0.64340(3) 0.04135(9) Uani 1 1 d . . .
Si1 Si 0.58643(7) 0.38209(6) 0.12820(6) 0.01555(13) Uani 1 1 d . . .
Si2 Si 0.33578(7) 0.25548(6) -0.09742(6) 0.01528(13) Uani 1 1 d . . .
Si3 Si 0.26610(7) 0.45064(6) -0.01872(6) 0.01587(13) Uani 1 1 d . . .
Si4 Si 0.51599(7) 0.57679(6) 0.20666(6) 0.01513(12) Uani 1 1 d . . .
O1 O 0.46565(18) 0.28194(16) 0.00713(15) 0.0175(3) Uani 1 1 d . . .
O2 O 0.28055(19) 0.33264(17) -0.04978(16) 0.0194(4) Uani 1 1 d . . .
O3 O 0.37684(18) 0.54041(16) 0.10917(16) 0.0173(3) Uani 1 1 d . . .
O4 O 0.54188(18) 0.46409(16) 0.18722(16) 0.0178(3) Uani 1 1 d . . .
O5 O 0.37210(18) 0.30241(16) -0.19767(16) 0.0177(3) Uani 1 1 d . . .
O6 O 0.29161(18) 0.52857(17) -0.10513(16) 0.0184(3) Uani 1 1 d . . .
C1 C 0.6316(3) 0.2948(2) 0.2185(2) 0.0182(5) Uani 1 1 d . . .
C2 C 0.5618(3) 0.1647(2) 0.1728(2) 0.0214(5) Uani 1 1 d . . .
H2A H 0.4932 0.1241 0.0976 0.026 Uiso 1 1 calc R . .
C3 C 0.5925(3) 0.0956(2) 0.2367(3) 0.0239(5) Uani 1 1 d . . .
C4 C 0.6914(3) 0.1507(3) 0.3465(3) 0.0263(6) Uani 1 1 d . . .
H4A H 0.7105 0.1016 0.3894 0.032 Uiso 1 1 calc R . .
C5 C 0.7621(3) 0.2787(3) 0.3931(2) 0.0237(5) Uani 1 1 d . . .
H5B H 0.8309 0.3186 0.4682 0.028 Uiso 1 1 calc R . .
C6 C 0.7315(3) 0.3481(2) 0.3288(2) 0.0189(5) Uani 1 1 d . . .
C7 C 0.1504(3) 0.0139(2) -0.1068(2) 0.0194(5) Uani 1 1 d . . .
C8 C 0.0521(3) -0.1088(3) -0.1621(3) 0.0258(6) Uani 1 1 d . . .
H8A H 0.0153 -0.1576 -0.1205 0.031 Uiso 1 1 calc R . .
C9 C 0.0075(3) -0.1604(2) -0.2791(3) 0.0256(6) Uani 1 1 d . . .
H9A H -0.0595 -0.2447 -0.3181 0.031 Uiso 1 1 calc R . .
C10 C 0.0621(3) -0.0869(2) -0.3374(2) 0.0191(5) Uani 1 1 d . . .
C11 C 0.1614(2) 0.0355(2) -0.2819(2) 0.0175(4) Uani 1 1 d . . .
H11A H 0.1978 0.0835 -0.3243 0.021 Uiso 1 1 calc R . .
C12 C 0.2091(2) 0.0896(2) -0.1636(2) 0.0161(4) Uani 1 1 d . . .
C13 C 0.1061(3) 0.3977(2) -0.0167(2) 0.0189(5) Uani 1 1 d . . .
C14 C -0.0117(3) 0.3007(3) -0.1037(2) 0.0241(5) Uani 1 1 d . . .
C15 C -0.1273(3) 0.2510(3) -0.0919(3) 0.0285(6) Uani 1 1 d . . .
H15A H -0.2061 0.1854 -0.1532 0.034 Uiso 1 1 calc R . .
C16 C -0.1261(3) 0.2985(3) 0.0103(3) 0.0279(6) Uani 1 1 d . . .
H16A H -0.2037 0.2647 0.0205 0.034 Uiso 1 1 calc R . .
C17 C -0.0107(3) 0.3955(3) 0.0973(2) 0.0230(5) Uani 1 1 d . . .
C18 C 0.1036(3) 0.4458(2) 0.0844(2) 0.0197(5) Uani 1 1 d . . .
H18A H 0.1812 0.5138 0.1449 0.024 Uiso 1 1 calc R . .
C19 C 0.5159(3) 0.6170(2) 0.3472(2) 0.0187(5) Uani 1 1 d . . .
C20 C 0.4170(3) 0.5391(3) 0.3736(2) 0.0239(5) Uani 1 1 d . . .
C21 C 0.4094(3) 0.5758(3) 0.4743(3) 0.0333(7) Uani 1 1 d . . .
H21A H 0.3393 0.5218 0.4886 0.040 Uiso 1 1 calc R . .
C22 C 0.5036(4) 0.6904(3) 0.5531(3) 0.0361(7) Uani 1 1 d . . .
H22A H 0.4985 0.7170 0.6217 0.043 Uiso 1 1 calc R . .
C23 C 0.6061(3) 0.7671(3) 0.5318(3) 0.0292(6) Uani 1 1 d . . .
C24 C 0.6116(3) 0.7324(3) 0.4297(2) 0.0227(5) Uani 1 1 d . . .
H24A H 0.6813 0.7876 0.4158 0.027 Uiso 1 1 calc R . .
S1 S 0.5440(4) 0.0395(4) 0.5404(3) 0.0715(9) Uani 0.50 1 d PDU A -1
S2 S 0.3241(3) -0.2183(3) 0.3689(2) 0.0673(7) Uani 0.50 1 d PDU A -1
C25 C 0.4333(9) -0.0957(6) 0.4493(9) 0.058(2) Uani 0.50 1 d PDU A -1
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'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O4 Si1 O6 109.56(10) . 2_665
O4 Si1 O1 109.00(10) . .
O6 Si1 O1 109.27(10) 2_665 .
O4 Si1 C1 111.46(11) . .
O6 Si1 C1 109.91(11) 2_665 .
O1 Si1 C1 107.59(11) . .
O2 Si2 O1 108.27(10) . .
O2 Si2 O5 108.82(10) . .
O1 Si2 O5 109.60(10) . .
O2 Si2 C12 110.23(11) . .
O1 Si2 C12 112.98(11) . .
O5 Si2 C12 106.88(10) . .
O2 Si3 O6 110.16(10) . .
O2 Si3 O3 108.28(11) . .
O6 Si3 O3 107.51(10) . .
O2 Si3 C13 109.02(11) . .
O6 Si3 C13 114.23(11) . .
O3 Si3 C13 107.44(11) . .
O4 Si4 O3 110.50(10) . .
O4 Si4 O5 109.43(10) . 2_665
O3 Si4 O5 107.96(10) . 2_665
O4 Si4 C19 111.90(11) . .
O3 Si4 C19 107.97(11) . .
O5 Si4 C19 108.98(11) 2_665 .
Si2 O1 Si1 144.10(13) . .
Si2 O2 Si3 155.88(13) . .
Si4 O3 Si3 144.18(13) . .
Si1 O4 Si4 153.96(13) . .
Si4 O5 Si2 137.47(12) 2_665 .
Si3 O6 Si1 137.83(13) . 2_665
C6 C1 C2 116.8(2) . .
C6 C1 Si1 124.93(19) . .
C2 C1 Si1 118.3(2) . .
C3 C2 C1 120.4(3) . .
C4 C3 C2 121.8(3) . .
C4 C3 Br2 119.5(2) . .
C2 C3 Br2 118.8(2) . .
C3 C4 C5 118.9(3) . .
C4 C5 C6 119.3(3) . .
C5 C6 C1 122.9(2) . .
C5 C6 Br1 117.1(2) . .
C1 C6 Br1 120.1(2) . .
C8 C7 C12 122.6(2) . .
C8 C7 Br3 116.9(2) . .
C12 C7 Br3 120.44(19) . .
C7 C8 C9 119.6(3) . .
C10 C9 C8 118.8(2) . .
C9 C10 C11 121.6(2) . .
C9 C10 Br4 119.5(2) . .
C11 C10 Br4 118.9(2) . .
C10 C11 C12 120.7(2) . .
C7 C12 C11 116.6(2) . .
C7 C12 Si2 125.28(19) . .
C11 C12 Si2 118.00(18) . .
C14 C13 C18 116.9(2) . .
C14 C13 Si3 124.3(2) . .
C18 C13 Si3 118.2(2) . .
C15 C14 C13 122.6(3) . .
C15 C14 Br5 117.4(2) . .
C13 C14 Br5 119.9(2) . .
C16 C15 C14 119.1(3) . .
C17 C16 C15 119.2(3) . .
C16 C17 C18 121.4(3) . .
C16 C17 Br6 119.7(2) . .
C18 C17 Br6 118.8(2) . .
C17 C18 C13 120.7(2) . .
C24 C19 C20 116.9(2) . .
C24 C19 Si4 120.4(2) . .
C20 C19 Si4 122.5(2) . .
C21 C20 C19 122.2(3) . .
C21 C20 Br7 117.6(2) . .
C19 C20 Br7 120.1(2) . .
C22 C21 C20 119.6(3) . .
C21 C22 C23 119.5(3) . .
C22 C23 C24 121.0(3) . .
C22 C23 Br8 120.1(2) . .
C24 C23 Br8 118.9(2) . .
C23 C24 C19 120.7(3) . .
S2 C25 S1 175.2(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C6 1.906(3) .
Br2 C3 1.902(3) .
Br3 C7 1.903(3) .
Br4 C10 1.896(3) .
Br5 C14 1.898(3) .
Br6 C17 1.890(3) .
Br7 C20 1.898(3) .
Br8 C23 1.887(3) .
Si1 O4 1.6139(19) .
Si1 O6 1.6212(19) 2_665
Si1 O1 1.6251(19) .
Si1 C1 1.852(3) .
Si2 O2 1.607(2) .
Si2 O1 1.619(2) .
Si2 O5 1.6285(19) .
Si2 C12 1.846(2) .
Si3 O2 1.609(2) .
Si3 O6 1.619(2) .
Si3 O3 1.6195(19) .
Si3 C13 1.850(3) .
Si4 O4 1.6157(19) .
Si4 O3 1.618(2) .
Si4 O5 1.6213(19) 2_665
Si4 C19 1.843(3) .
O5 Si4 1.6213(19) 2_665
O6 Si1 1.6212(19) 2_665
C1 C6 1.393(4) .
C1 C2 1.408(3) .
C2 C3 1.383(4) .
C3 C4 1.382(4) .
C4 C5 1.387(4) .
C5 C6 1.388(4) .
C7 C8 1.383(4) .
C7 C12 1.397(3) .
C8 C9 1.391(4) .
C9 C10 1.379(4) .
C10 C11 1.384(3) .
C11 C12 1.406(3) .
C13 C14 1.394(4) .
C13 C18 1.399(4) .
C14 C15 1.391(4) .
C15 C16 1.386(4) .
C16 C17 1.382(4) .
C17 C18 1.384(4) .
C19 C24 1.396(4) .
C19 C20 1.400(4) .
C20 C21 1.388(4) .
C21 C22 1.371(5) .
C22 C23 1.384(5) .
C23 C24 1.385(4) .
S1 C25 1.608(7) .
S2 C25 1.473(7) .
