A Molecular Balloon: Expansion of a Molecular Gyrotop Cage Due to Rotation of the Phenylene Rotor
Wataru Setaka; Kentaro Yamaguchi; Journal of the American Chemical Society 134 (2012) 12458–12461; doi:10.1021/ja305822e

data_4118449
_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'
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.1046P)^2^+3.7358P] where P=(Fo^2^+2Fc^2^)/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     >2\s(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