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_7246142
_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         'C33 H32 Cd2 O14, 2(H2 O)'
_chemical_formula_sum            'C33 H36 Cd2 O16'
_chemical_formula_weight         913.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-21
_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                67.884(4)
_cell_angle_beta                 86.175(3)
_cell_angle_gamma                82.860(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7940(3)
_cell_length_b                   14.7078(6)
_cell_length_c                   15.9272(6)
_cell_measurement_reflns_used    8903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9900
_cell_measurement_theta_min      2.6120
_cell_volume                     1677.93(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_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   -101.00  24.00   0.50    6.00    --  -11.20 -60.00  90.00  250
  2  \w   -101.00  24.00   0.50    6.00    --  -11.20 -60.00-120.00  250
  3  \w   -101.00  78.00   0.50    6.00    --  -11.20   0.00-150.00  358
  4  \w   -101.00  24.00   0.50    6.00    --  -11.20 -60.00   0.00  250
  5  \w    -55.00  78.00   0.50    6.00    --  -11.20  41.00-125.55  266
  6  \w    -47.00  -8.00   0.50    6.00    --  -11.20  60.00  30.00   78
  7  \w    -47.00  78.00   0.50    6.00    --  -11.20  57.00 -30.00  250
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38564
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.390
_exptl_absorpt_coefficient_mu    1.345
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019)
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    1.808
_exptl_crystal_description       plate
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.451
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7689
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0503P)^2^+4.8301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6284
_reflns_number_total             7689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01552h2.cif
_cod_data_source_block           2020ep374_a_1a
_cod_depositor_comments
'Adding full bibliography for 7246140--7246143.cif.'
_cod_database_code               7246142
_shelx_shelxl_version_number     2018/3
_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, All O(H,H) groups
2. Restrained distances
 O17-H17C = O17-H17D
 0.84 with sigma of 0.01
 H17D-O5_$2
 1.9 with sigma of 0.02
 H17C-H17D
 1.33 with sigma of 0.02
 Cd2-H14A \\sim Cd2-H14B
 with sigma of 0.02
3.a Free rotating group:
 O14(H14A,H14B), O16(H16D,H16E), O17(H17C,H17D)
3.b Rotating group:
 O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B), O12(H12A,H12B), O13(H13A,H13B)
3.c Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
3.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C11(H11), C12(H12), C14(H14), C21(H21), C24(H24),
 C25(H25), C28(H28), C29(H29), C32(H32)
3.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              76030
_shelx_hkl_checksum              26674
_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
;