Synthesis of Crystalline Molecular Gyrotops and Phenylene Rotation inside the Cage.
Setaka, Wataru; Inoue, Kazuyuki; Higa, Sayaka; Yoshigai, Seiki; Kono, Hirohiko; Yamaguchi, Kentaro; The Journal of organic chemistry 79 (2014) 8288–8295; doi:10.1021/jo501539h

data_4029857
_publ_section_title
;
 Synthesis of Crystalline Molecular Gyrotops and Phenylene Rotation inside
 the Cage.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8288
_journal_page_last               8295
_journal_paper_doi               10.1021/jo501539h
_journal_volume                  79
_journal_year                    2014
_chemical_formula_moiety         'C54 H100 Si2'
_chemical_formula_sum            'C54 H100 Si2'
_chemical_formula_weight         805.51
_chemical_melting_point          416.8(3)
_chemical_name_common            C16MolGyro
_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_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 121.13(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.51(6)
_cell_length_b                   12.34(2)
_cell_length_c                   17.98(4)
_cell_measurement_reflns_used    664
_cell_measurement_temperature    270(2)
_cell_measurement_theta_max      13.16
_cell_measurement_theta_min      2.51
_cell_volume                     5415(19)
_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      270(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0420
_diffrn_reflns_av_unetI/netI     0.0944
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12083
_diffrn_reflns_point_group_measured_fraction_full 0.828
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.669
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS  Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.988
_exptl_crystal_description       plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.150
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 410 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.69(19)
_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     505
_refine_ls_number_reflns         7911
_refine_ls_number_restraints     499
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.3938
_refine_ls_R_factor_gt           0.1216
_refine_ls_shift/su_max          0.930
_refine_ls_shift/su_mean         0.172
_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          0.3025
_refine_ls_wR_factor_ref         0.4879
_reflns_Friedel_coverage         0.660
_reflns_Friedel_fraction_full    0.658
_reflns_Friedel_fraction_max     0.658
_reflns_number_gt                1267
_reflns_number_total             7911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo501539h_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '143.3-143.9 degC' was changed to
'416.8(3)' - 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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4029857.cif.
;
_cod_original_cell_volume        5414(18)
_cod_database_code               4029857
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.992