6,6'-Biindeno[1,2-<i>b</i>]fluorene: an open-shell indenofluorene dimer.
Sharma, Himanshu; Jana, Palash; Mallick, Dibyendu; Bandyopadhyay, Subhajit; Das, Soumyajit; Chemical science 15 (2024) 20215–20222; doi:10.1039/d4sc03996c

data_1573191
_publ_section_title
;
 6,6'-Biindeno[1,2-<i>b</i>]fluorene: an open-shell indenofluorene dimer.
;
_journal_issue                   48
_journal_name_full               'Chemical science'
_journal_page_first              20215
_journal_page_last               20222
_journal_paper_doi               10.1039/d4sc03996c
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C58 H42'
_chemical_formula_sum            'C58 H42'
_chemical_formula_weight         738.980
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_Int_Tables_number      4
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.474(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.265(3)
_cell_length_b                   8.009(2)
_cell_length_c                   19.200(4)
_cell_measurement_reflns_used    5269
_cell_measurement_temperature    298
_cell_measurement_theta_max      24.834
_cell_measurement_theta_min      2.773
_cell_volume                     2103.5(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.9984
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_Laue_measured_fraction_full 0.9983
_diffrn_reflns_Laue_measured_fraction_max 0.9984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35051
_diffrn_reflns_point_group_measured_fraction_full 0.9990
_diffrn_reflns_point_group_measured_fraction_max 0.9990
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.21
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1231 before and 0.0813 after correction.
The Ratio of minimum to maximum transmission is 0.7798.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       needle
_exptl_crystal_F_000             780.400
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'slow solvent diffusion of methanol into DCM/carbon disulfide (1:1) solution'
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.4236
_refine_diff_density_min         -0.2896
_refine_diff_density_rms         0.0582
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   8(6)
_refine_ls_d_res_high            0.8200
_refine_ls_d_res_low             9.2057
_refine_ls_goodness_of_fit_ref   1.0448
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     529
_refine_ls_number_reflns         7972
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0448
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.1651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1569
_reflns_Friedel_coverage         1.000
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              9
_reflns_limit_k_min              -9
_reflns_limit_l_max              23
_reflns_limit_l_min              -23
_reflns_number_gt                5137
_reflns_number_total             7972
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4sc03996c2.cif
_cod_data_source_block           SDHS_6_0m
_cod_depositor_comments          'Adding full bibliography for 1573191.cif.'
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               1573191
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C21(H21), C27(H27), C2(H2), C57(H57), C38(H38), C35(H35), C54(H54),
 C34(H34), C33(H33), C53(H53), C52(H52), C51(H51), C7(H7), C44(H44), C14(H14),
 C5(H5), C8(H8), C47(H47), C6(H6), C26(H26), C17(H17), C24(H24), C25(H25)
2.b Idealised Me refined as rotating group:
 C43(H43a,H43b,H43c), C19(H19a,H19b,H19c), C49(H49a,H49b,H49c), C13(H13a,H13b,
 H13c), C16(H16a,H16b,H16c), C46(H46a,H46b,H46c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'