Intermolecular interactions in molecular crystals and their effect on thermally activated delayed fluorescence of helicene-based emitters
Klimash, Anastasia; Pander, Piotr; Klooster, Wim T.; Coles, Simon J.; Data, Przemyslaw; Dias, Fernando B.; Skabara, Peter J.; Journal of Materials Chemistry C 6 (2018) 10557–; doi:10.1039/C8TC03390K

data_7237475
_publ_section_title
;
 Intermolecular interactions in molecular crystals and their effect on
 thermally activated delayed fluorescence of helicene-based emitters
;
_journal_issue                   39
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              10557
_journal_paper_doi               10.1039/C8TC03390K
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C44 H26 N4 O2'
_chemical_formula_sum            'C44 H26 N4 O2'
_chemical_formula_weight         642.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-03 deposited with the CCDC.
2018-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 136.902(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.514(2)
_cell_length_b                   9.0508(3)
_cell_length_c                   19.0317(16)
_cell_measurement_reflns_used    11119
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.7780
_cell_measurement_theta_min      2.0890
_cell_volume                     3002.8(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_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      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_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    -24.00  93.00   0.50   10.00    --    3.30  57.00 -90.00  234
  2  \w    -24.00  93.00   0.50   10.00    --    3.30  57.00-180.00  234
  3  \w    -93.00  24.00   0.50   10.00    --   -3.60 -57.00 -30.00  234
  4  \w    -40.00  86.00   0.50   10.00    --   -3.60  19.00 -60.00  252
  5  \w    -29.00  86.00   0.50   10.00    --   -3.60  38.00  90.00  230
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0064141000
_diffrn_orient_matrix_UB_12      0.0668993000
_diffrn_orient_matrix_UB_13      0.0248013000
_diffrn_orient_matrix_UB_21      -0.0390234000
_diffrn_orient_matrix_UB_22      0.0008653000
_diffrn_orient_matrix_UB_23      -0.0275928000
_diffrn_orient_matrix_UB_31      0.0096500000
_diffrn_orient_matrix_UB_32      -0.0407921000
_diffrn_orient_matrix_UB_33      0.0399827000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33178
_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         27.484
_diffrn_reflns_theta_min         2.141
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       needle
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+3.0616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3095
_reflns_number_total             3451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8tc03390k2.cif
_cod_data_source_block           2017ncs0734a
_cod_original_cell_volume        3002.7(7)
_cod_database_code               7237475
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C44 H26 N4 O2'
_chemical_oxdiff_usercomment     NKH1PXZneedles
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C17(H00B), C5(H00C), C2(H00D), C22(H00E), C3(H00F), C18(H00H), C10(H00J),
 C11(H00K), C9(H00L), C4(H00M), C15(H00N), C8(H00O), C16(H00P)
;
_shelx_res_checksum              48587
_shelx_hkl_checksum              22457
_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 3.556
_oxdiff_exptl_absorpt_empirical_full_min 0.431