#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:36:02 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178955 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/84/4118449.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_4118449
loop_
_publ_author_name
'Wataru Setaka'
'Kentaro Yamaguchi'
_publ_section_title
;
 A Molecular Balloon: Expansion of a Molecular Gyrotop Cage Due to
 Rotation of the Phenylene Rotor
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12458
_journal_page_last               12461
_journal_paper_doi               10.1021/ja305822e
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C48 H82 Si2'
_chemical_formula_sum            'C48 H82 Si2'
_chemical_formula_weight         715.32
_chemical_melting_point          475(1)
_chemical_name_common            'A Molecular Gyrotop'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 123.1930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.8310(10)
_cell_length_b                   10.9710(10)
_cell_length_c                   16.5240(10)
_cell_measurement_reflns_used    18053
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.68
_cell_measurement_theta_min      2.71
_cell_volume                     4525.5(5)
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_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 19.5
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.747
_diffrn_measurement.details
' 1.00 degrees, 30.0 sec, detector distance 75.00 mm'
_diffrn_measurement_device_type  'Rigaku/MSC Jupiter210 CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_source         'SPring-8 BL38B2 beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5482
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.68
_diffrn_reflns_theta_min         2.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9978
_exptl_absorpt_correction_T_min  0.9978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL SCALEPACK'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_description       prism
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.023(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         5482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0674
_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)+(0.1046P)²+3.7358P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.1909
_reflns_number_gt                4770
_reflns_number_total             5482
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ja305822e_si_002.cif
_cod_data_source_block           MolGyrotop2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4118449
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
C01 C 0.94294(7) -0.01756(15) 0.19867(11) 0.0391(4) Uani 1 1 d .
C02 C 0.97222(6) 0.09108(16) 0.22429(11) 0.0413(4) Uani 1 1 d .
H02 H 0.9536 0.1666 0.2061 0.050 Uiso 1 1 calc R
C03 C 0.97211(6) -0.12608(16) 0.22539(11) 0.0413(4) Uani 1 1 d .
H03 H 0.9536 -0.2016 0.2097 0.050 Uiso 1 1 calc R
C04 C 0.83814(7) -0.16443(16) 0.07589(12) 0.0423(4) Uani 1 1 d .
H04A H 0.8531 -0.2271 0.1274 0.051 Uiso 1 1 calc R
H04B H 0.7991 -0.1608 0.0472 0.051 Uiso 1 1 calc R
C05 C 0.84704(7) -0.20651(17) -0.00211(12) 0.0428(4) Uani 1 1 d .
H05A H 0.8861 -0.2105 0.0260 0.051 Uiso 1 1 calc R
H05B H 0.8317 -0.1449 -0.0544 0.051 Uiso 1 1 calc R
C06 C 0.82226(7) -0.33096(17) -0.04614(13) 0.0476(4) Uani 1 1 d .
H06A H 0.7830 -0.3254 -0.0776 0.057 Uiso 1 1 calc R
H06B H 0.8291 -0.3498 -0.0970 0.057 Uiso 1 1 calc R
C07 C 0.84322(8) -0.43580(18) 0.02589(13) 0.0502(4) Uani 1 1 d .
H07A H 0.8260 -0.5123 -0.0093 0.060 Uiso 1 1 calc R
H07B H 0.8327 -0.4219 0.0726 0.060 Uiso 1 1 calc R
C08 C 0.90372(8) -0.45137(18) 0.08152(13) 0.0506(4) Uani 1 1 d .
H08A H 0.9208 -0.3789 0.1231 0.061 Uiso 1 1 calc R
H08B H 0.9146 -0.4541 0.0347 0.061 Uiso 1 1 calc R
C09 C 0.92491(9) -0.56503(19) 0.14464(15) 0.0588(5) Uani 1 1 d .
H09A H 0.9124 -0.5656 0.1891 0.071 Uiso 1 1 calc R
H09B H 0.9103 -0.6383 0.1031 0.071 Uiso 1 1 calc R
C10 C 0.98439(9) -0.57029(18) 0.20213(14) 0.0578(5) Uani 1 1 d .
H10 H 1.0014 -0.5739 0.1675 0.069 Uiso 1 1 calc R
C11 C 0.84394(7) 0.10941(18) 0.03980(12) 0.0460(4) Uani 1 1 d .
H11A H 0.8507 0.1893 0.0724 0.055 Uiso 1 1 calc R
H11B H 0.8658 0.1061 0.0115 0.055 Uiso 1 1 calc R
C12 C 0.78495(7) 0.10361(18) -0.04256(13) 0.0467(4) Uani 1 1 d .
H12A H 0.7791 0.0302 -0.0821 0.056 Uiso 1 1 calc R
H12B H 0.7630 0.0947 -0.0147 0.056 Uiso 1 1 calc R
C13 C 0.76571(7) 0.21521(19) -0.10815(13) 0.0511(5) Uani 1 1 d .
H13A H 0.7270 0.2058 -0.1580 0.061 Uiso 1 1 calc R
H13B H 0.7700 0.2881 -0.0691 0.061 Uiso 1 1 calc R
C14 C 0.79492(8) 0.2364(2) -0.15757(14) 0.0555(5) Uani 1 1 d .
H14A H 0.7875 0.1671 -0.2016 0.067 Uiso 1 1 calc R
H14B H 0.8339 0.2369 -0.1079 0.067 Uiso 1 1 calc R
C15 C 0.78024(8) 0.35456(19) -0.21572(13) 0.0518(5) Uani 1 1 d .
H15A H 0.7424 0.3503 -0.2709 0.062 Uiso 1 1 calc R
H15B H 0.7836 0.4237 -0.1742 0.062 Uiso 1 1 calc R
C16 C 0.81567(9) 0.3776(2) -0.25360(14) 0.0587(5) Uani 1 1 d .
H16A H 0.8126 0.3078 -0.2943 0.070 Uiso 1 1 calc R
H16B H 0.8028 0.4513 -0.2950 0.070 Uiso 1 1 calc R
C17 C 0.87279(8) 0.3949(2) -0.17516(15) 0.0566(5) Uani 1 1 d .
H17 H 0.8817 0.4648 -0.1353 0.068 Uiso 1 1 calc R
C18 C 0.91224(8) 0.3210(2) -0.15632(14) 0.0544(5) Uani 1 1 d .
H18 H 0.9034 0.2534 -0.1985 0.065 Uiso 1 1 calc R
C19 C 0.96918(8) 0.3333(2) -0.07560(15) 0.0568(5) Uani 1 1 d .
H19A H 0.9723 0.3994 -0.0320 0.068 Uiso 1 1 calc R
H19B H 0.9907 0.3569 -0.1022 0.068 Uiso 1 1 calc R
C20 C 0.99224(8) 0.2157(2) -0.01695(14) 0.0532(5) Uani 1 1 d .
H20A H 0.9684 0.1867 0.0034 0.064 Uiso 1 1 calc R
H20B H 0.9931 0.1521 -0.0585 0.064 Uiso 1 1 calc R
C21 C 1.04808(7) 0.23330(18) 0.07161(13) 0.0475(4) Uani 1 1 d .
H21A H 1.0462 0.2894 0.1166 0.057 Uiso 1 1 calc R
H21B H 1.0705 0.2726 0.0518 0.057 Uiso 1 1 calc R
C22 C 1.07498(7) 0.11581(17) 0.12476(12) 0.0454(4) Uani 1 1 d .
H22A H 1.0807 0.0631 0.0825 0.054 Uiso 1 1 calc R
H22B H 1.0510 0.0719 0.1389 0.054 Uiso 1 1 calc R
C23 C 1.12850(7) 0.13868(18) 0.21885(13) 0.0465(4) Uani 1 1 d .
H23A H 1.1234 0.2005 0.2568 0.056 Uiso 1 1 calc R
H23B H 1.1537 0.1729 0.2036 0.056 Uiso 1 1 calc R
C24 C 1.15380(7) 0.02395(17) 0.28170(13) 0.0454(4) Uani 1 1 d .
H24A H 1.1932 0.0341 0.3204 0.054 Uiso 1 1 calc R
H24B H 1.1453 -0.0467 0.2383 0.054 Uiso 1 1 calc R
Si01 Si 0.867810(17) -0.01316(4) 0.13356(3) 0.03895(19) Uani 1 1 d .
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'
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
C03 C01 C02 116.94(15) . .
C03 C01 Si01 122.93(13) . .
C02 C01 Si01 120.11(12) . .
C02 C02 C01 121.57(10) 2_755 .
C02 C02 H02 119.2 2_755 .
C01 C02 H02 119.2 . .
C03 C03 C01 121.47(10) 2_755 .
C03 C03 H03 119.3 2_755 .
C01 C03 H03 119.3 . .
C05 C04 Si01 116.45(12) . .
C05 C04 H04A 108.2 . .
Si01 C04 H04A 108.2 . .
C05 C04 H04B 108.2 . .
Si01 C04 H04B 108.2 . .
H04A C04 H04B 107.3 . .
C04 C05 C06 114.16(15) . .
C04 C05 H05A 108.7 . .
C06 C05 H05A 108.7 . .
C04 C05 H05B 108.7 . .
C06 C05 H05B 108.7 . .
H05A C05 H05B 107.6 . .
C07 C06 C05 114.64(14) . .
C07 C06 H06A 108.6 . .
C05 C06 H06A 108.6 . .
C07 C06 H06B 108.6 . .
C05 C06 H06B 108.6 . .
H06A C06 H06B 107.6 . .
C06 C07 C08 113.65(16) . .
C06 C07 H07A 108.8 . .
C08 C07 H07A 108.8 . .
C06 C07 H07B 108.8 . .
C08 C07 H07B 108.8 . .
H07A C07 H07B 107.7 . .
C07 C08 C09 114.58(17) . .
C07 C08 H08A 108.6 . .
C09 C08 H08A 108.6 . .
C07 C08 H08B 108.6 . .
C09 C08 H08B 108.6 . .
H08A C08 H08B 107.6 . .
C10 C09 C08 111.85(17) . .
C10 C09 H09A 109.2 . .
C08 C09 H09A 109.2 . .
C10 C09 H09B 109.2 . .
C08 C09 H09B 109.2 . .
H09A C09 H09B 107.9 . .
C10 C10 C09 125.1(3) 2_755 .
C10 C10 H10 117.4 2_755 .
C09 C10 H10 117.4 . .
C12 C11 Si01 115.99(13) . .
C12 C11 H11A 108.3 . .
Si01 C11 H11A 108.3 . .
C12 C11 H11B 108.3 . .
Si01 C11 H11B 108.3 . .
H11A C11 H11B 107.4 . .
C13 C12 C11 113.71(16) . .
C13 C12 H12A 108.8 . .
C11 C12 H12A 108.8 . .
C13 C12 H12B 108.8 . .
C11 C12 H12B 108.8 . .
H12A C12 H12B 107.7 . .
C14 C13 C12 113.94(16) . .
C14 C13 H13A 108.8 . .
C12 C13 H13A 108.8 . .
C14 C13 H13B 108.8 . .
C12 C13 H13B 108.8 . .
H13A C13 H13B 107.7 . .
C13 C14 C15 114.89(17) . .
C13 C14 H14A 108.5 . .
C15 C14 H14A 108.5 . .
C13 C14 H14B 108.5 . .
C15 C14 H14B 108.5 . .
H14A C14 H14B 107.5 . .
C16 C15 C14 112.14(17) . .
C16 C15 H15A 109.2 . .
C14 C15 H15A 109.2 . .
C16 C15 H15B 109.2 . .
C14 C15 H15B 109.2 . .
H15A C15 H15B 107.9 . .
C17 C16 C15 112.81(16) . .
C17 C16 H16A 109.0 . .
C15 C16 H16A 109.0 . .
C17 C16 H16B 109.0 . .
C15 C16 H16B 109.0 . .
H16A C16 H16B 107.8 . .
C18 C17 C16 125.3(2) . .
C18 C17 H17 117.3 . .
C16 C17 H17 117.3 . .
C17 C18 C19 126.2(2) . .
C17 C18 H18 116.9 . .
C19 C18 H18 116.9 . .
C18 C19 C20 112.89(18) . .
C18 C19 H19A 109.0 . .
C20 C19 H19A 109.0 . .
C18 C19 H19B 109.0 . .
C20 C19 H19B 109.0 . .
H19A C19 H19B 107.8 . .
C21 C20 C19 112.35(17) . .
C21 C20 H20A 109.1 . .
C19 C20 H20A 109.1 . .
C21 C20 H20B 109.1 . .
C19 C20 H20B 109.1 . .
H20A C20 H20B 107.9 . .
C20 C21 C22 113.89(16) . .
C20 C21 H21A 108.8 . .
C22 C21 H21A 108.8 . .
C20 C21 H21B 108.8 . .
C22 C21 H21B 108.8 . .
H21A C21 H21B 107.7 . .
C21 C22 C23 112.22(16) . .
C21 C22 H22A 109.2 . .
C23 C22 H22A 109.2 . .
C21 C22 H22B 109.2 . .
C23 C22 H22B 109.2 . .
H22A C22 H22B 107.9 . .
C22 C23 C24 114.02(15) . .
C22 C23 H23A 108.7 . .
C24 C23 H23A 108.7 . .
C22 C23 H23B 108.7 . .
C24 C23 H23B 108.7 . .
H23A C23 H23B 107.6 . .
C23 C24 Si01 115.97(13) . 2_755
C23 C24 H24A 108.3 . .
Si01 C24 H24A 108.3 2_755 .
C23 C24 H24B 108.3 . .
Si01 C24 H24B 108.3 2_755 .
H24A C24 H24B 107.4 . .
C11 Si01 C04 110.78(8) . .
C11 Si01 C24 109.31(9) . 2_755
C04 Si01 C24 108.12(8) . 2_755
C11 Si01 C01 106.60(8) . .
C04 Si01 C01 110.52(8) . .
C24 Si01 C01 111.51(8) 2_755 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C01 C03 1.396(2) .
C01 C02 1.399(2) .
C01 Si01 1.8823(17) .
C02 C02 1.388(3) 2_755
C02 H02 0.9500 .
C03 C03 1.396(3) 2_755
C03 H03 0.9500 .
C04 C05 1.523(2) .
C04 Si01 1.8768(18) .
C04 H04A 0.9900 .
C04 H04B 0.9900 .
C05 C06 1.533(2) .
C05 H05A 0.9900 .
C05 H05B 0.9900 .
C06 C07 1.522(3) .
C06 H06A 0.9900 .
C06 H06B 0.9900 .
C07 C08 1.521(3) .
C07 H07A 0.9900 .
C07 H07B 0.9900 .
C08 C09 1.523(3) .
C08 H08A 0.9900 .
C08 H08B 0.9900 .
C09 C10 1.486(3) .
C09 H09A 0.9900 .
C09 H09B 0.9900 .
C10 C10 1.326(4) 2_755
C10 H10 0.9500 .
C11 C12 1.527(2) .
C11 Si01 1.8728(18) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.524(3) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.503(3) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 C15 1.528(3) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C16 1.516(3) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 C17 1.484(3) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.318(3) .
C17 H17 0.9500 .
C18 C19 1.484(3) .
C18 H18 0.9500 .
C19 C20 1.532(3) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 C21 1.511(2) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 C22 1.518(3) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 C23 1.520(2) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 C24 1.541(3) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 Si01 1.8790(19) 2_755
C24 H24A 0.9900 .
C24 H24B 0.9900 .
Si01 C24 1.8790(19) 2_755
