Isomeric Dibenzooctazethrene Diradicals for High-Performance Air-Stable Organic Field-Effect Transistors
Zong, Chaoyang; Yang, Shuyuan; Sun, Yajing; Zhang, Lifeng; Hu, Jinlian; Hu, Wenping; Li, Rongjin; Sun, Zhe; Chemical Science  (2022) –; doi:10.1039/D2SC03667C

data_1567628
_publ_section_title
;
 Isomeric Dibenzooctazethrene Diradicals for High-Performance Air-Stable
 Organic Field-Effect Transistors
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC03667C
_journal_year                    2022
_chemical_formula_moiety         'C32 H33 Si'
_chemical_formula_sum            'C64 H66 Si2'
_chemical_formula_weight         445.704
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc285mrv
_audit_creation_date             2021-06-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.05.01 svn.r6f5a8f70 for OlexSys, GUI svn.r6320)
;
_audit_update_record
;
2021-06-18 deposited with the CCDC.	2022-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.080(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2848(5)
_cell_length_b                   7.9227(1)
_cell_length_c                   19.2800(6)
_cell_measurement_reflns_used    6046
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      73.6640
_cell_measurement_theta_min      2.7550
_cell_volume                     2486.81(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9550
_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    -31.00  -5.00   0.50    0.19    --  -47.00  47.00 -89.00   52
  2  \w    -99.00 -69.00   0.50    0.19    --  -47.00 -47.00 121.00   60
  3  \w     36.00 118.00   0.50    0.19    --   47.00  47.00 -89.00  164
  4  \w    -24.00  63.00   0.50    0.19    --   47.00 -47.00 121.00  174
  5  \w   -100.00 -74.00   0.50    0.78    -- -100.00  47.00 -89.00   52
  6  \w   -131.00-105.00   0.50    0.78    -- -100.00 -47.00 121.00   52
  7  \w     93.00 156.00   0.50    0.78    --  107.61  47.00 -89.00  126
  8  \w     36.00 121.00   0.50    0.78    --  107.61 -47.00 121.00  170
  9  \w    -95.00 -26.00   0.50    0.19    --  -47.00 125.00-120.00  138
 10  \w     84.00 109.00   0.50    0.19    --   47.00 125.00-150.00   50
 11  \w   -114.00 -24.00   0.50    0.78    -- -100.00  19.00 120.00  180
 12  \w   -114.00 -45.00   0.50    0.78    -- -100.00  37.00 120.00  138
 13  \w   -170.00-101.00   0.50    0.78    -- -100.00 -99.00-150.00  138
 14  \w    145.00 173.00   0.50    0.78    --  107.61  19.00 150.00   56
 15  \w     98.00 143.00   0.50    0.78    --  107.61  19.00 150.00   90
 16  \w     93.00 175.00   0.50    0.78    --  107.61  37.00-120.00  164
 17  \w     51.00 124.00   0.50    0.78    --  107.61 -57.00   0.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0515700000
_diffrn_orient_matrix_UB_12      0.1075608000
_diffrn_orient_matrix_UB_13      0.0726314000
_diffrn_orient_matrix_UB_21      0.0634089000
_diffrn_orient_matrix_UB_22      0.0319621000
_diffrn_orient_matrix_UB_23      -0.0304288000
_diffrn_orient_matrix_UB_31      -0.0477021000
_diffrn_orient_matrix_UB_32      0.1587850000
_diffrn_orient_matrix_UB_33      -0.0431083000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9550
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16506
_diffrn_reflns_point_group_measured_fraction_full 0.9991
_diffrn_reflns_point_group_measured_fraction_max 0.9550
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.59
_diffrn_reflns_theta_min         2.76
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             959.375
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.3614
_refine_diff_density_min         -0.2992
_refine_diff_density_rms         0.0657
_refine_ls_d_res_high            0.7925
_refine_ls_d_res_low             15.9952
_refine_ls_goodness_of_fit_ref   1.0285
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    52
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0285
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+0.6043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1526
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -22
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              -11
_reflns_number_gt                3938
_reflns_number_total             4983
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2sc03667c2.cif
_cod_data_source_block           exp_255
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1567628
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00G(H00G), C00M(H00M), C00Q(H00Q)
2.b Aromatic/amide H refined with riding coordinates:
 C006(H006), C007(H007), C00I(H00I), C00K(H00K), C00L(H00L), C00N(H00N),
 C00O(H00O), C00R(H00R), C00S(H00S)
2.c Idealised Me refined as rotating group:
 C00J(H00a,H00b,H00c), C00P(H00d,H00e,H00f), C00T(H00h,H00j,H00p), C00U(H00t,
 H00u,H00v), C00V(H00w,H00x,H00y), C00W(H00z,H,Ha), C00X(H00,Hb,Hc)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 3.091
_oxdiff_exptl_absorpt_empirical_full_min 0.436