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_4129054
_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         'C52 H30 Cl6'
_chemical_formula_sum            'C52 H30 Cl6'
_chemical_formula_weight         867.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 108.122(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.0733(3)
_cell_length_b                   23.6070(5)
_cell_length_c                   11.7842(2)
_cell_measurement_reflns_used    11788
_cell_measurement_temperature    123
_cell_measurement_theta_max      73.53
_cell_measurement_theta_min      4.34
_cell_volume                     3985.24(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            32262
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.274
_diffrn_reflns_theta_min         3.609
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.229
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            clearcolourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776.00
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     560
_refine_ls_number_reflns         7976
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1178P)^2^+4.9879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6990
_reflns_number_total             7976
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja9b09179_si_005.cif
_cod_data_source_block           xcalibur
_cod_database_code               4129054
_shelx_res_checksum              30800
_shelx_hkl_checksum              95227