Order-Disorder Transition of Dipolar Rotor in a Crystalline Molecular Gyrotop and Its Optical Change
Wataru Setaka; Kentaro Yamaguchi; Journal of the American Chemical Society 135 (2013) 14560–14563; doi:10.1021/ja408405f

data_4120908
_publ_contact_author_address     'Tokyo Metropolitan University, Japan'
_publ_contact_author_email       wsetaka@tmu.ac.jp
_publ_contact_author_name        'Wataru Setaka'
_publ_contact_author_phone       +81-42-677-1111
_publ_section_title
;
 Order-Disorder Transition of Dipolar Rotor in a Crystalline Molecular
 Gyrotop and Its Optical Change
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14560
_journal_page_last               14563
_journal_paper_doi               10.1021/ja408405f
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C46 H86 S Si2'
_chemical_formula_sum            'C46 H86 S Si2'
_chemical_formula_weight         727.39
_chemical_melting_point          423(1)
_chemical_name_common            'Thiophene-bridged Gyrotop'
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 122.538(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.546(9)
_cell_length_b                   12.446(5)
_cell_length_c                   18.039(7)
_cell_measurement_reflns_used    829
_cell_measurement_temperature    270(2)
_cell_measurement_theta_max      15.27
_cell_measurement_theta_min      2.59
_cell_volume                     4835(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      270(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11610
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.27
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.9788
_exptl_absorpt_correction_T_min  0.8854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS  Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.999
_exptl_crystal_description       plate
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7288
_refine_ls_number_restraints     365
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.3347
_refine_ls_R_factor_gt           0.1187
_refine_ls_shift/su_max          0.907
_refine_ls_shift/su_mean         0.163
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2792
_refine_ls_wR_factor_ref         0.4280
_reflns_number_gt                1516
_reflns_number_total             7288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408405f_si_003.cif
_cod_data_source_block           ThioGyro270K
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4120908