A Crystalline Molecular Gyrotop with a Biphenylene Dirotor and its Temperature Dependent Birefringence
Fujiwara, Atsushi; Inagaki, Yusuke; Momma, Hiroyuki; Kwon, Eunsang; Yamaguchi, Kentaro; Kanno, Manabu; Kono, Hirohiko; Setaka, Wataru; CrystEngComm  (2017) –; doi:10.1039/C7CE01081H

data_7229170
_publ_section_title
;
 A Crystalline Molecular Gyrotop with a Biphenylene Dirotor and its
 Temperature Dependent Birefringence
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01081H
_journal_year                    2017
_chemical_compound_source        no
_chemical_formula_moiety         'C66 H116 Si2'
_chemical_formula_sum            'C66 H116 Si2'
_chemical_formula_weight         965.76
_chemical_melting_point          "'274-276 deg.C'"
_chemical_name_common            C18satBiphCage
_chemical_name_systematic        C18satBiphCage
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1p5yyr
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.8090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.097(3)
_cell_length_b                   11.4728(10)
_cell_length_c                   16.9361(14)
_cell_measurement_reflns_used    3969
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      2.48
_cell_volume                     6374.7(9)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.917
_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  0.0242
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17101
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.932
_diffrn_reflns_theta_min         1.241
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.006
_exptl_crystal_description       prism
_exptl_crystal_F_000             2160
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran/methanol (4:1 v/v)'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         7008
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1516P)^2^+5.6586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2458
_refine_ls_wR_factor_ref         0.2783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4602
_reflns_number_total             7008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01081h2.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_cell_volume        6374.6(9)
_cod_database_code               7229170
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.995
_shelxl_version_number           2013-4
_shelx_res_checksum              65942