Open-shell singlet diradicaloid difluoreno[4,3-b:3',4'-d]furan and its radical cation and dianion.
Mori, Sakura; Akita, Motoko; Suzuki, Shuichi; Asano, Motoko S.; Murata, Michihisa; Akiyama, Tsuyoshi; Matsumoto, Taisuke; Kitamura, Chitoshi; Kato, Shin-Ichiro; Chemical communications (Cambridge, England) 56 (2020) 5881–5884; doi:10.1039/d0cc01638a

data_7126430
_publ_section_title
;
 Open-shell singlet diradicaloid difluoreno[4,3-b:3',4'-d]furan and its
 radical cation and dianion.
;
_journal_issue                   44
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5881
_journal_page_last               5884
_journal_paper_doi               10.1039/d0cc01638a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C44 H34 O'
_chemical_formula_sum            'C44 H34 O'
_chemical_formula_weight         578.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-28 deposited with the CCDC.	2020-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.127(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0514(2)
_cell_length_b                   29.7733(7)
_cell_length_c                   12.8449(3)
_cell_measurement_reflns_used    12618
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.6230
_cell_measurement_theta_min      2.0670
_cell_volume                     3077.02(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -5.00  21.00   0.50    3.00    --  -15.50  45.00  90.00   52
  2  \w    -99.00 -73.00   0.50    3.00    --  -15.50  45.00  60.00   52
  3  \w    -61.00  49.00   0.50    3.00    --  -15.50  45.00  60.00  220
  4  \w   -104.00  68.00   0.50    3.00    --  -15.50  45.00   0.00  344
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0071763000
_diffrn_orient_matrix_UB_12      -0.0050126000
_diffrn_orient_matrix_UB_13      -0.0539837000
_diffrn_orient_matrix_UB_21      -0.0873211000
_diffrn_orient_matrix_UB_22      -0.0023075000
_diffrn_orient_matrix_UB_23      0.0036593000
_diffrn_orient_matrix_UB_31      -0.0099585000
_diffrn_orient_matrix_UB_32      0.0231576000
_diffrn_orient_matrix_UB_33      -0.0113485000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24852
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.095
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              FR-E+
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+1.0846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6041
_reflns_number_total             7055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01638a2.cif
_cod_data_source_block           ks1811f
_cod_depositor_comments          'Adding full bibliography for 7126430.cif.'
_cod_database_code               7126430
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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:
 C8(H8), C9(H9), C18(H18), C4(H4), C15(H15), C5(H5), C21(H21), C29(H29),
 C24(H24), C16(H16), C23(H23), C17(H17), C22(H22), C40(H40), C31(H31), C38(H38)
2.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C35(H35A,H35B,
 H35C), C34(H34A,H34B,H34C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              12963
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.825