On the role of torsional dynamics in the solid-state fluorescent properties of a new bifluorene–tetracarboxylic acid and its supramolecular assemblies: a structural and TD-DFT investigation
Podda, Enrico; Arca, Massimiliano; Pintus, Anna; Lippolis, Vito; Caltagirone, Claudia; Coles, Simon J.; Orton, James B.; Ennas, Guido; Picci, Giacomo; Davies, Robert P.; Aragoni, M. Carla; CrystEngComm 25 (2023) 1058–1066; doi:10.1039/D2CE01552H

data_7246143
_publ_section_title
;
 On the role of torsional dynamics in the solid-state fluorescent
 properties of a new bifluorene--tetracarboxylic acid and its
 supramolecular assemblies: a structural and TD-DFT investigation
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1058
_journal_page_last               1066
_journal_paper_doi               10.1039/D2CE01552H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C29 H20 Br4'
_chemical_formula_sum            'C29 H20 Br4'
_chemical_formula_weight         688.09
_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     dual
_audit_creation_date             2022-10-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-21 deposited with the CCDC.	2023-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.0820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.79840(10)
_cell_length_b                   16.7929(2)
_cell_length_c                   16.4790(2)
_cell_measurement_reflns_used    29133
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.5510
_cell_measurement_theta_min      2.3210
_cell_volume                     2410.60(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_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    -99.00  24.00   0.50    0.50    --   -9.80 -57.00  90.00  246
  2  \w    -99.00  27.00   0.50    0.50    --   -9.80 -70.00 -90.00  252
  3  \w    -99.00  58.00   0.50    0.50    --   -9.80 -19.00 -60.00  314
  4  \w    -46.00  80.00   0.50    0.50    --   -9.80  70.00  30.00  252
  5  \w    -84.00  42.00   0.50    0.50    --    5.00 -38.00-180.00  252
  6  \w    -47.00   9.00   0.50    0.50    --   -9.80  38.00 -30.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54497
_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         2.338
_exptl_absorpt_coefficient_mu    6.695
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.271
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.18b (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             1336
_exptl_crystal_recrystallization_method
'The material was recrystallised from acetone'
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+1.9005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5047
_reflns_number_total             5543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01552h2.cif
_cod_data_source_block           2018ncs0887r1
_cod_depositor_comments
'Adding full bibliography for 7246140--7246143.cif.'
_cod_database_code               7246143
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.500
_shelx_estimated_absorpt_t_min   0.210
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C19(H19), C21(H21),
 C22(H22), C25(H25), C26(H26), C28(H28)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              99148
_shelx_hkl_checksum              86884
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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
;