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_7229171
_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          548.1(10)
_chemical_name_common            C18BiPhcage
_chemical_name_systematic        C18BiPhcage
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1p5yzs
_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                 120.161(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.52(3)
_cell_length_b                   10.968(9)
_cell_length_c                   19.057(16)
_cell_measurement_reflns_used    963
_cell_measurement_temperature    280(2)
_cell_measurement_theta_max      15.04
_cell_measurement_theta_min      2.51
_cell_volume                     6600(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      280(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Bruker SMART 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  0.0377
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17562
_diffrn_reflns_point_group_measured_fraction_full 0.830
_diffrn_reflns_point_group_measured_fraction_max 0.731
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.775
_diffrn_reflns_theta_min         1.290
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.972
_exptl_crystal_description       plate
_exptl_crystal_F_000             2160
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran/methanol=4:1'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.126
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 709 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.46(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         11397
_refine_ls_number_restraints     653
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.3565
_refine_ls_R_factor_gt           0.1208
_refine_ls_shift/su_max          1.439
_refine_ls_shift/su_mean         0.296
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3104
_refine_ls_wR_factor_ref         0.4710
_reflns_Friedel_coverage         0.598
_reflns_Friedel_fraction_full    0.663
_reflns_Friedel_fraction_max     0.547
_reflns_number_gt                2038
_reflns_number_total             11397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01081h2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '274-276 deg.C' was changed to
'548.1(10)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        6600(10)
_cod_database_code               7229171
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.974
_shelxl_version_number           2013-4
_shelx_res_checksum              93929