Linear [3]Spirobifluorenylene: An S-Shaped Molecular Geometry of <i>p</i>-Oligophenyls.
Oniki, Jumpei; Moriuchi, Toshiyuki; Kamochi, Kosuke; Tobisu, Mamoru; Amaya, Toru; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b09179

data_4129053
_publ_section_title
;
 Linear [3]Spirobifluorenylene: An S-Shaped Molecular Geometry of
 <i>p</i>-Oligophenyls.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b09179
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C75 H40, 2.5(C7 H8)'
_chemical_formula_sum            'C92.5 H60'
_chemical_formula_weight         1171.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_audit_creation_date             2019-7-12
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 94.1993(5)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.80350(10)
_cell_length_b                   44.6481(2)
_cell_length_c                   33.5757(2)
_cell_measurement_reflns_used    115284
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      76.3200
_cell_measurement_theta_min      3.7030
_cell_volume                     25122.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     35.00 121.00   0.50    0.85    --   47.45  37.00  90.00  172
  2  \w     70.00  95.00   0.50    3.40    --   70.50  83.00 -48.00   50
  3  \w     58.00  95.00   0.50    3.40    --   70.50  37.00  30.00   74
  4  \w     26.00 110.00   0.50    0.85    --   47.45  83.00 -48.00  168
  5  \w     71.00 120.00   0.50    0.85    --   47.45 125.00  60.00   98
  6  \w    -23.00  61.00   0.50    0.85    --   47.45 -57.00-150.00  168
  7  \w     17.00  73.00   0.50    0.85    --   47.45 -83.00-169.00  112
  8  \w     23.00  48.00   0.50    3.40    --   70.50 -83.00-169.00   50
  9  \w     11.00  94.00   0.50    0.85    --   47.45-125.00  30.00  166
 10  \w    -48.00 -23.00   0.50    0.85    --  -47.45  83.00 -48.00   50
 11  \w    -69.00 -34.00   0.50    3.40    -- -106.00 125.00   0.00   70
 12  \w   -116.00 -91.00   0.50    3.40    -- -106.00 125.00   0.00   50
 13  \w   -131.00 -49.00   0.50    3.40    -- -106.00  83.00 -48.00  164
 14  \w    -93.00 -40.00   0.50    3.40    -- -106.00 125.00-180.00  106
 15  \w   -120.00 -34.00   0.50    3.40    -- -106.00  57.00 -30.00  172
 16  \w   -124.00 -91.00   0.50    3.40    -- -106.00 -57.00-120.00   66
 17  \w   -139.00-104.00   0.50    3.40    -- -106.00 -37.00 -90.00   70
 18  \w    -71.00 -45.00   0.50    0.85    --  -47.45 -83.00-169.00   52
 19  \w    -97.00 -49.00   0.50    3.40    -- -106.00 125.00 150.00   96
 20  \w   -154.00 -94.00   0.50    3.40    -- -106.00 -37.00  60.00  120
 21  \w   -119.00 -86.00   0.50    3.40    -- -106.00 -99.00  60.00   66
 22  \w   -118.00 -74.00   0.50    0.85    --  -47.45-125.00 -30.00   88
 23  \w   -120.00 -71.00   0.50    0.85    --  -47.45-125.00   0.00   98
 24  \w   -164.00-138.00   0.50    3.40    -- -106.00 -57.00-120.00   52
 25  \w   -168.00-124.00   0.50    3.40    -- -106.00 -37.00 -60.00   88
 26  \w   -170.00 -80.00   0.50    3.40    -- -106.00 -83.00-169.00  180
 27  \w   -171.00 -98.00   0.50    3.40    -- -106.00 -37.00-120.00  146
 28  \w   -177.00 -84.00   0.50    3.40    -- -106.00 -77.00-150.00  186
 29  \w   -168.00-104.00   0.50    3.40    -- -106.00 -19.00  30.00  128
 30  \w   -175.00 -93.00   0.50    3.40    -- -106.00 -37.00 120.00  164
 31  \w   -175.00-104.00   0.50    3.40    -- -106.00 -19.00  90.00  142
 32  \w   -177.00-147.00   0.50    3.40    -- -106.00 -37.00 -90.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            157913
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.710
_diffrn_reflns_theta_min         3.300
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             9840
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.133
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 22004 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.9(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3537
_refine_ls_number_reflns         50550
_refine_ls_number_restraints     409
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0782P)^2^+18.6515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                48875
_reflns_number_total             50550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09179_si_003.cif
_cod_data_source_block           190614_jo_02_116_rsr_c75h40
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C92.50 H60'
_cod_database_code               4129053
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.705
_oxdiff_exptl_absorpt_empirical_full_max 1.359
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_hkl_checksum              22198