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_7237474
_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, C6 H14'
_chemical_formula_sum            'C50 H40 N4 O2'
_chemical_formula_weight         728.86
_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             2017-11-07
_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                 97.5790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.28030(10)
_cell_length_b                   14.5794(2)
_cell_length_c                   22.9364(2)
_cell_measurement_reflns_used    24466
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.3050
_cell_measurement_theta_min      5.8450
_cell_volume                     3739.17(7)
_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(1)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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    -89.00  89.00   0.50    0.50    --    0.00  14.00 -60.00  356
  2  \w    -89.00  89.00   0.50    0.50    --    0.00  60.00-180.00  356
  3  \w   -179.00  -1.00   0.50    0.50    --  -90.00  43.00   0.00  356
  4  \w   -179.00  -1.00   0.50    0.50    --  -90.00  60.00-180.00  356
  5  \w   -179.00  -1.00   0.50    0.50    --  -90.00  60.00 -60.00  356
  6  \w   -179.00  -1.00   0.50    0.50    --  -90.00  43.00  30.00  356
  7  \w   -179.00  -1.00   0.50    0.50    --  -90.00  57.00  30.00  356
  8  \w   -179.00  -1.00   0.50    0.50    --  -90.00  60.00 -30.00  356
  9  \w   -179.00 -43.00   0.50    0.50    --  -90.00  60.00  90.00  272
 10  \w   -178.00-142.00   0.50    0.50    --  -90.00  60.00-150.00   72
 11  \w   -136.00 -22.00   0.50    0.50    --  -90.00  60.00-150.00  228
 12  \w    -69.00  -1.00   0.50    0.50    --  -90.00  57.00 -90.00  136
 13  \w   -172.00 -48.00   0.50    0.50    --  -90.00  60.00   0.00  248
 14  \w   -179.00-153.00   0.50    0.50    --  -90.00  60.00  60.00   52
 15  \w   -147.00-104.00   0.50    0.50    --  -90.00  60.00  60.00   86
 16  \w   -153.00-111.00   0.50    0.50    --  -90.00   0.00-180.00   84
 17  \w    -65.00 -39.00   0.50    0.50    --  -90.00   0.00-180.00   52
 18  \w   -174.00-139.00   0.50    0.50    --  -90.00  60.00 120.00   70
 19  \w   -179.00  -1.00   0.50    0.50    --  -90.00  60.00-120.00  356
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type  'DOT HyPix'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0051840000
_diffrn_orient_matrix_UB_12      0.0458011000
_diffrn_orient_matrix_UB_13      0.0601488000
_diffrn_orient_matrix_UB_21      -0.1339319000
_diffrn_orient_matrix_UB_22      -0.0236986000
_diffrn_orient_matrix_UB_23      -0.0041521000
_diffrn_orient_matrix_UB_31      0.0317692000
_diffrn_orient_matrix_UB_32      -0.0922782000
_diffrn_orient_matrix_UB_33      0.0308804000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31606
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.235
_diffrn_reflns_theta_min         6.376
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87279
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0445
_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^)+(0.0416P)^2^+4.4809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3305
_reflns_number_total             3349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8tc03390k2.cif
_cod_data_source_block           2017ncs0714a
_cod_database_code               7237474
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C44 H26 N4 O2'
_chemical_oxdiff_usercomment     NKH1PXZ
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.886
_reflns_odcompleteness_completeness 97.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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:
 C24(H24A,H24B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C18(H18), C15(H15), C11(H11), C17(H17), C2(H2), C16(H16), C8(H8),
 C10(H10), C5(H5), C9(H9), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C)
;
_shelx_res_checksum              88353
_shelx_hkl_checksum              96649
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id NKH1PXZ
_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 1.325
_oxdiff_exptl_absorpt_empirical_full_min 0.818