The impact of film deposition and annealing on the nanostructure and dielectric constant of organic semiconductor thin films.
Packman, Lachlan; Mallo, Neil; Raynor, Aaron; Gao, Mile; Babazadeh, Mohammad; Jin, Hui; Huang, David M.; Burn, Paul L.; Gentle, Ian R.; Shaw, Paul E.; Physical chemistry chemical physics : PCCP 25 (2023) 23867–23878; doi:10.1039/d3cp03038e

data_7247257
_publ_section_title
;
 The impact of film deposition and annealing on the nanostructure and
 dielectric constant of organic semiconductor thin films.
;
_journal_issue                   35
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              23867
_journal_page_last               23878
_journal_paper_doi               10.1039/d3cp03038e
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C46 H50 N4 O8 S4'
_chemical_formula_sum            'C46 H50 N4 O8 S4'
_chemical_formula_weight         915.14
_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             2021-11-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-06-26 deposited with the CCDC.	2023-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.437(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2402(4)
_cell_length_b                   10.7034(5)
_cell_length_c                   22.9820(12)
_cell_measurement_reflns_used    7985
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.8570
_cell_measurement_theta_min      2.6050
_cell_volume                     2253.83(19)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.999
_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     -8.00  78.00   0.50   15.00    --    8.20  57.00  90.00  172
  2  \w     -2.00  46.00   0.50   15.00    --    8.20 -99.00 -60.00   96
  3  \w    -10.00  16.00   0.50   15.00    --   -9.60  23.00-158.00   52
  4  \w      6.00  45.00   0.50   15.00    --    8.20 -99.00 120.00   78
  5  \w    -65.00  -3.00   0.50   15.00    --   -9.60 -23.00  36.00  124
  6  \w    -73.00  11.00   0.50   15.00    --   -9.60 -77.00 -30.00  168
  7  \w    -63.00   9.00   0.50   15.00    --    8.20 -57.00-180.00  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0373480000
_diffrn_orient_matrix_UB_12      0.0097546000
_diffrn_orient_matrix_UB_13      0.0285789000
_diffrn_orient_matrix_UB_21      0.0664149000
_diffrn_orient_matrix_UB_22      -0.0186149000
_diffrn_orient_matrix_UB_23      -0.0098740000
_diffrn_orient_matrix_UB_31      0.0137938000
_diffrn_orient_matrix_UB_32      0.0628502000
_diffrn_orient_matrix_UB_33      -0.0073344000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29935
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         2.611
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0618P)^2^+3.9023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4455
_reflns_number_total             5606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp03038e2.cif
_cod_data_source_block           splb19jc01
_cod_depositor_comments          'Adding full bibliography for 7247257.cif.'
_cod_database_code               7247257
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C92 H92 N8 O16 S8 '
_chemical_oxdiff_usercomment     Aaron
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.974
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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:
 C14(H14A,H14B), C19(H19A,H19B), C15(H15A,H15B), C20(H20A,H20B), C17(H17A,
 H17B), C16(H16A,H16B), C22(H22A,H22B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C8(H8), C4(H4)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              62583
_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 1.472
_oxdiff_exptl_absorpt_empirical_full_min 0.691