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_4129055
_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_formula_moiety         'C75 H40, 6(C7 H8)'
_chemical_formula_sum            'C117 H88'
_chemical_formula_weight         1493.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_audit_creation_date             2018-10-24
_audit_creation_method
'generated by ACTA instruction via SHELXL-2014/7'
_cell_angle_alpha                88.1162(14)
_cell_angle_beta                 78.2974(12)
_cell_angle_gamma                80.0559(11)
_cell_formula_units_Z            2
_cell_length_a                   9.95880(10)
_cell_length_b                   18.0963(3)
_cell_length_c                   23.5648(4)
_cell_measurement_reflns_used    39441
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.2510
_cell_measurement_theta_min      3.8040
_cell_volume                     4096.03(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_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 0.999
_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    -24.00  68.00   0.50    1.20    --   42.80 -73.00  77.00  184
  2  \w     29.00  54.00   0.50    4.81    --   76.50 -73.00  77.00   50
  3  \w     20.00  77.00   0.50    4.81    --   76.50 -37.00-120.00  114
  4  \w     17.00 107.00   0.50    1.20    --   42.80  73.00-153.00  180
  5  \w     75.00 100.00   0.50    4.81    --   76.50  73.00-153.00   50
  6  \w    107.00 148.00   0.50    4.81    --   76.50 125.00-150.00   82
  7  \w     75.00 117.00   0.50    1.20    --   42.80 125.00  90.00   84
  8  \w     71.00 150.00   0.50    4.81    --   76.50 125.00 120.00  158
  9  \w     -3.00  23.00   0.50    1.20    --  -42.80  73.00-153.00   52
 10  \w    -53.00 -26.00   0.50    1.20    --  -42.80  73.00-153.00   54
 11  \w    -88.00 -41.00   0.50    4.81    -- -106.00  73.00-153.00   94
 12  \w    -77.00 -43.00   0.50    4.81    -- -106.00 125.00-180.00   68
 13  \w    -92.00 -66.00   0.50    4.81    -- -106.00 125.00-120.00   52
 14  \w   -109.00 -38.00   0.50    4.81    -- -106.00 125.00-150.00  142
 15  \w    -95.00 -15.00   0.50    1.20    --  -42.80 125.00-180.00  160
 16  \w    -64.00 -33.00   0.50    4.81    -- -106.00 125.00 -30.00   62
 17  \w    -72.00 -46.00   0.50    4.81    -- -106.00  37.00  30.00   52
 18  \w    -69.00 -37.00   0.50    4.81    -- -106.00  19.00  90.00   64
 19  \w    -77.00 -33.00   0.50    4.81    -- -106.00  57.00 150.00   88
 20  \w    -84.00 -56.00   0.50    4.81    -- -106.00  77.00 150.00   56
 21  \w    -94.00 -68.00   0.50    4.81    -- -106.00  77.00  90.00   52
 22  \w   -120.00 -42.00   0.50    4.81    -- -106.00 125.00  60.00  156
 23  \w   -120.00 -88.00   0.50    4.81    -- -106.00 125.00 -60.00   64
 24  \w   -119.00 -71.00   0.50    4.81    -- -106.00 125.00 -30.00   96
 25  \w   -128.00 -34.00   0.50    4.81    -- -106.00  57.00  60.00  188
 26  \w   -117.00 -78.00   0.50    4.81    -- -106.00  37.00  30.00   78
 27  \w   -135.00 -64.00   0.50    4.81    -- -106.00  77.00 -60.00  142
 28  \w    -89.00 -25.00   0.50    4.81    -- -106.00  19.00-120.00  128
 29  \w   -104.00 -78.00   0.50    4.81    -- -106.00 -77.00-120.00   52
 30  \w   -138.00-104.00   0.50    4.81    -- -106.00  19.00-120.00   68
 31  \w   -134.00 -39.00   0.50    4.81    -- -106.00  77.00-180.00  190
 32  \w   -115.00 -89.00   0.50    4.81    -- -106.00 125.00-180.00   52
 33  \w   -135.00 -32.00   0.50    4.81    -- -106.00  77.00  30.00  206
 34  \w   -127.00-102.00   0.50    4.81    -- -106.00  77.00 150.00   50
 35  \w   -127.00 -85.00   0.50    4.81    -- -106.00  57.00 150.00   84
 36  \w   -138.00 -74.00   0.50    4.81    -- -106.00  19.00  90.00  128
 37  \w   -107.00 -17.00   0.50    1.20    --  -42.80 -73.00  77.00  180
 38  \w   -113.00 -83.00   0.50    4.81    -- -106.00 -99.00 150.00   60
 39  \w   -159.00-124.00   0.50    4.81    -- -106.00 -99.00 150.00   70
 40  \w   -166.00 -90.00   0.50    4.81    -- -106.00 -73.00  77.00  152
 41  \w   -149.00 -88.00   0.50    4.81    -- -106.00 -99.00 -60.00  122
 42  \w   -158.00-125.00   0.50    4.81    -- -106.00 -37.00-180.00   66
 43  \w   -154.00-129.00   0.50    4.81    -- -106.00 -77.00-120.00   50
 44  \w   -177.00-107.00   0.50    4.81    -- -106.00 -57.00   0.00  140
 45  \w   -173.00-121.00   0.50    4.81    -- -106.00 -37.00 150.00  104
 46  \w   -169.00-107.00   0.50    4.81    -- -106.00 -57.00  90.00  124
 47  \w   -119.00 -62.00   0.50    4.81    -- -106.00 125.00 120.00  114
 48  \w   -113.00 -36.00   0.50    4.81    -- -106.00 125.00 150.00  154
;
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            59132
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.499
_diffrn_reflns_theta_max         67.499
_diffrn_reflns_theta_min         3.831
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         14729
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.1070
_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^)+(0.0201P)^2^+17.1354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2314
_refine_ls_wR_factor_ref         0.2350
_reflns_number_gt                14092
_reflns_number_total             14729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09179_si_002.cif
_cod_data_source_block           exp133
_cod_database_code               4129055
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              67949
_shelx_hkl_checksum              98156