#------------------------------------------------------------------------------
#$Date: 2016-03-26 12:56:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180217 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/03/7110340.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_7110340
loop_
_publ_author_name
'Wataru Setak'
'Soichiro Ohmizu'
'Mitsuo Kira'
_publ_section_title
;
 Kinetic stabilization against the oxidation reaction induced by a
 silaalkane cage in a thiophene-bridged molecular gyroscope
;
_journal_name_full               Chem.Commun.
_journal_page_first              1098
_journal_paper_doi               10.1039/c3cc48205g
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         '(C52 H122 O5 S Si14), 3(C4H8O)'
_chemical_formula_sum            'C64 H146 O8 S Si14'
_chemical_formula_weight         1469.13
_chemical_name_common            SO2-bridged_molecular_gyroscope_with_3THF
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   26.249(2)
_cell_length_b                   26.249(2)
_cell_length_c                   22.827(4)
_cell_measurement_reflns_used    3629
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      1.55
_cell_volume                     13621(3)
_computing_cell_refinement       'APEX 2 Bruker'
_computing_data_collection       'APEX 2 Bruker'
_computing_data_reduction        'APEX 2 Bruker'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25260
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.9494
_exptl_absorpt_correction_T_min  0.9023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS  Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4836
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0528
_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)+(0.0874P)²+31.5013P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                3049
_reflns_number_total             3629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc48205g.txt
_cod_data_source_block           SO2THF
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7110340
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'
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
S1 S 0.69442(7) 0.3333 0.0833 0.0246(4) Uani 0.33 2 d SP
Si1 Si 0.6667 0.3333 0.22244(4) 0.0230(2) Uani 1 3 d S
Si2 Si 0.86445(2) 0.40348(3) 0.24829(3) 0.03228(19) Uani 1 1 d .
Si3 Si 0.90387(3) 0.50077(3) 0.07272(3) 0.03369(19) Uani 1 1 d .
O1 O 0.7493(2) 0.3874(2) 0.0808(3) 0.0455(13) Uani 0.33 1 d P
O2 O 0.86638(16) 0.53305(16) 0.0833 0.0702(10) Uani 1 2 d S
C1 C 0.6852(3) 0.3491(4) 0.1414(2) 0.0236(12) Uani 0.33 1 d P
C2 C 0.7301(3) 0.3960(3) 0.1158(2) 0.0301(13) Uani 0.33 1 d P
H2 H 0.7606 0.4268 0.1379 0.036 Uiso 0.33 1 calc PR
C3 C 0.74449(9) 0.38089(9) 0.24663(11) 0.0342(5) Uani 1 1 d .
H3A H 0.7617 0.4188 0.2253 0.041 Uiso 1 1 calc R
H3B H 0.7448 0.3895 0.2889 0.041 Uiso 1 1 calc R
C4 C 0.78353(9) 0.35317(9) 0.23640(10) 0.0330(4) Uani 1 1 d .
H4A H 0.7775 0.3383 0.1957 0.040 Uiso 1 1 calc R
H4B H 0.7700 0.3189 0.2629 0.040 Uiso 1 1 calc R
C5 C 0.89216(9) 0.46382(9) 0.19299(9) 0.0332(4) Uani 1 1 d .
H5A H 0.8719 0.4867 0.1990 0.040 Uiso 1 1 calc R
H5B H 0.9347 0.4907 0.1998 0.040 Uiso 1 1 calc R
C6 C 0.88310(13) 0.44246(11) 0.12873(11) 0.0472(6) Uani 1 1 d .
H6A H 0.8411 0.4126 0.1232 0.057 Uiso 1 1 calc R
H6B H 0.9064 0.4228 0.1218 0.057 Uiso 1 1 calc R
C7 C 0.87888(12) 0.43492(15) 0.32329(11) 0.0538(7) Uani 1 1 d .
H7A H 0.8642 0.4030 0.3521 0.081 Uiso 1 1 calc R
H7B H 0.8588 0.4575 0.3287 0.081 Uiso 1 1 calc R
H7C H 0.9213 0.4608 0.3287 0.081 Uiso 1 1 calc R
C8 C 0.90239(12) 0.35968(13) 0.23810(14) 0.0543(7) Uani 1 1 d .
H8A H 0.8946 0.3430 0.1985 0.081 Uiso 1 1 calc R
H8B H 0.8875 0.3278 0.2670 0.081 Uiso 1 1 calc R
H8C H 0.9449 0.3854 0.2434 0.081 Uiso 1 1 calc R
C9 C 0.98249(13) 0.5553(2) 0.07897(17) 0.0931(15) Uani 1 1 d .
H9A H 0.9931 0.5861 0.0494 0.140 Uiso 1 1 calc R
H9B H 1.0057 0.5360 0.0727 0.140 Uiso 1 1 calc R
H9C H 0.9906 0.5729 0.1181 0.140 Uiso 1 1 calc R
C10 C 0.88616(17) 0.46728(15) -0.00159(12) 0.0637(8) Uani 1 1 d .
H10A H 0.8440 0.4388 -0.0041 0.096 Uiso 1 1 calc R
H10B H 0.9085 0.4472 -0.0089 0.096 Uiso 1 1 calc R
H10C H 0.8966 0.4982 -0.0310 0.096 Uiso 1 1 calc R
O3 O 0.9443(3) 0.3333 0.0833 0.178(3) Uani 1 2 d S
C11 C 1.0020(3) 0.3790(3) 0.1023(4) 0.168(4) Uani 1 1 d .
H11A H 1.0107 0.4173 0.0854 0.202 Uiso 1 1 calc R
H11B H 1.0028 0.3825 0.1455 0.202 Uiso 1 1 calc R
C12 C 1.0460(3) 0.3647(3) 0.0834(5) 0.200(5) Uani 1 1 d .
H12A H 1.0608 0.3805 0.0437 0.240 Uiso 1 1 calc R
H12B H 1.0795 0.3804 0.1110 0.240 Uiso 1 1 calc R
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'
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
O1 S1 O1 118.7(5) . 16_554
O1 S1 C1 109.6(5) 16_554 .
O1 S1 C1 109.6(5) . 16_554
C1 S1 C1 143.8(8) . 16_554
O1 S1 C1 117.8(4) 16_554 18_544
C1 S1 C1 128.8(2) . 18_544
O1 S1 C1 117.8(4) . 3_665
C1 S1 C1 128.8(2) 16_554 3_665
C1 S1 C1 136.3(9) 18_544 3_665
S1 S1 C2 120.3(3) 2_655 16_554
O1 S1 C2 134.9(4) . 16_554
C1 S1 C2 131.6(4) . 16_554
C1 S1 C2 100.7(3) 3_665 16_554
S1 S1 C2 119.2(3) 3_665 18_544
O1 S1 C2 139.1(4) 16_554 18_544
C1 S1 C2 102.4(4) . 18_544
C1 S1 C2 132.3(3) 3_665 18_544
C2 S1 C2 124.9(4) 16_554 18_544
O1 S1 C2 139.1(4) . 3_665
C1 S1 C2 102.4(4) 16_554 3_665
C1 S1 C2 132.3(3) 18_544 3_665
O1 S1 C1 109.8(4) . 17_654
O1 S1 C1 109.7(5) 16_554 17_654
C1 S1 C1 119.2(6) . 17_654
C1 S1 C1 113.8(6) 3_665 17_654
C2 S1 C1 110.1(5) 3_665 17_654
C3 Si1 C3 111.64(7) 3_665 .
C3 Si1 C3 111.64(7) 3_665 2_655
C3 Si1 C3 111.64(7) . 2_655
C3 Si1 C1 110.3(4) . 3_665
C3 Si1 C1 116.6(3) 2_655 3_665
C3 Si1 C1 116.6(3) 3_665 .
C3 Si1 C1 110.3(4) 2_655 .
C3 Si1 C1 110.3(4) 3_665 2_655
C3 Si1 C1 116.6(3) . 2_655
C7 Si2 C5 109.91(13) . .
C7 Si2 C8 109.53(15) . .
C5 Si2 C8 109.62(11) . .
C7 Si2 C4 110.72(11) . .
C5 Si2 C4 108.85(10) . .
C8 Si2 C4 108.17(12) . .
O2 Si3 C9 108.9(2) . .
O2 Si3 C6 109.07(13) . .
C9 Si3 C6 109.97(15) . .
O2 Si3 C10 108.23(13) . .
C9 Si3 C10 110.92(19) . .
C6 Si3 C10 109.74(14) . .
Si3 O2 Si3 175.1(3) 18_544 .
C1 C1 C2 133.5(19) 2_655 .
C1 C1 C2 147.8(14) 3_665 .
C1 C1 S1 101.3(4) 2_655 .
C2 C1 S1 105.7(4) . 3_665
C1 C1 Si1 78.09(13) 2_655 .
C1 C1 Si1 78.09(13) 3_665 .
C2 C1 Si1 129.4(4) . .
S1 C1 Si1 152.9(8) . .
S1 C1 Si1 146.1(7) 2_655 .
S1 C1 Si1 124.6(3) 3_665 .
C1 C2 C2 115.9(3) . 18_544
C1 C2 H2 122.1 . .
C2 C2 H2 122.1 18_544 .
C4 C3 Si1 113.74(14) . .
C4 C3 H3A 108.8 . .
Si1 C3 H3A 108.8 . .
C4 C3 H3B 108.8 . .
Si1 C3 H3B 108.8 . .
H3A C3 H3B 107.7 . .
C3 C4 Si2 115.54(14) . .
C3 C4 H4A 108.4 . .
Si2 C4 H4A 108.4 . .
C3 C4 H4B 108.4 . .
Si2 C4 H4B 108.4 . .
H4A C4 H4B 107.5 . .
C6 C5 Si2 114.22(16) . .
C6 C5 H5A 108.7 . .
Si2 C5 H5A 108.7 . .
C6 C5 H5B 108.7 . .
Si2 C5 H5B 108.7 . .
H5A C5 H5B 107.6 . .
C5 C6 Si3 115.24(17) . .
C5 C6 H6A 108.5 . .
Si3 C6 H6A 108.5 . .
C5 C6 H6B 108.5 . .
Si3 C6 H6B 108.5 . .
H6A C6 H6B 107.5 . .
Si2 C7 H7A 109.5 . .
Si2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Si2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
Si2 C8 H8A 109.5 . .
Si2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
Si2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
Si3 C9 H9A 109.5 . .
Si3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
Si3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
Si3 C10 H10A 109.5 . .
Si3 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
Si3 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C11 O3 C11 101.8(8) . 16_554
C12 C11 O3 109.6(6) . .
C12 C11 H11A 109.8 . .
O3 C11 H11A 109.8 . .
C12 C11 H11B 109.8 . .
O3 C11 H11B 109.8 . .
H11A C11 H11B 108.2 . .
C12 C12 C11 103.0(4) 16_554 .
C12 C12 H12A 111.2 16_554 .
C11 C12 H12A 111.2 . .
C12 C12 H12B 111.2 16_554 .
C11 C12 H12B 111.2 . .
H12A C12 H12B 109.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 S1 1.262(3) 2_655
S1 S1 1.262(3) 3_665
S1 O1 1.431(5) .
S1 O1 1.431(5) 16_554
S1 C1 1.444(7) .
S1 C1 1.444(7) 16_554
S1 C1 1.498(8) 18_544
S1 C1 1.498(8) 3_665
S1 C2 1.609(6) 16_554
S1 C2 1.623(6) 18_544
S1 C2 1.623(6) 3_665
S1 C1 1.774(5) 17_654
Si1 C3 1.867(2) 3_665
Si1 C3 1.867(2) .
Si1 C3 1.867(2) 2_655
Si1 C1 1.905(6) 3_665
Si1 C1 1.905(6) .
Si1 C1 1.905(6) 2_655
Si2 C7 1.856(3) .
Si2 C5 1.865(2) .
Si2 C8 1.874(3) .
Si2 C4 1.877(2) .
Si3 O2 1.606(4) .
Si3 C9 1.837(3) .
Si3 C6 1.855(3) .
Si3 C10 1.860(3) .
O1 C2 0.965(8) 18_544
O1 O1 1.300(12) 18_544
O1 S1 1.919(5) 2_655
O2 Si3 1.606(4) 18_544
C1 C1 0.786(8) 2_655
C1 C1 0.786(8) 3_665
C1 C2 1.340(8) .
C1 S1 1.498(8) 2_655
C1 S1 1.774(5) 3_665
C2 C2 1.483(11) 18_544
C2 H2 0.9500 .
C3 C4 1.543(3) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.546(3) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
O3 C11 1.451(8) .
O3 C11 1.451(8) 16_554
C11 C12 1.447(10) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C12 1.428(14) 16_554
C12 H12A 0.9900 .
C12 H12B 0.9900 .
