A novel angularly fused bistetracene: facile synthesis, crystal packing and single-crystal field effect transistors
Zunzhi Wang; Rongjin Li; Yulan Chen; Yuan-Zhi Tan; Zeyi Tu; Xuejiao J. Gao; Huanli Dong; Yuanping Yi; Yu Zhang; Wenping Hu; Klaus Mullen; Long Chen; Journal of Materials Chemistry C 5 (2017) 1308–1312; doi:10.1039/C6TC04365H

data_7235170
_publ_section_title
;
 A novel angularly fused bistetracene: facile synthesis, crystal packing
 and single-crystal field effect transistors
;
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              1308
_journal_page_last               1312
_journal_paper_doi               10.1039/C6TC04365H
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         'C74 H96 Si4'
_chemical_formula_sum            'C74 H96 Si4'
_chemical_formula_weight         1097.87
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                81.367(8)
_cell_angle_beta                 85.995(8)
_cell_angle_gamma                80.270(9)
_cell_formula_units_Z            1
_cell_length_a                   7.4917(7)
_cell_length_b                   12.6697(14)
_cell_length_c                   17.4733(16)
_cell_measurement_reflns_used    1887
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      65.5580
_cell_measurement_theta_min      4.0920
_cell_volume                     1614.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega -114.00  -18.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6231  -57.0000   30.0000 96

  2 omega  -71.00   -8.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6231  125.0000 -120.0000 63

  3 omega  -49.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6231   38.0000 -180.0000 82

  4 omega   27.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6231 -125.0000 -180.0000 44

  5 omega   85.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7300   61.0000   30.0000 73

  6 omega   33.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7300 -125.0000  -30.0000 80

  7 omega   16.00   42.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7300  -30.0000  150.0000 26

  8 omega   71.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7300  -94.0000   60.0000 37

  9 omega  105.00  153.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7300  125.0000 -120.0000 48

 10 omega   89.00  164.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7300   45.0000  150.0000 75

 11 omega  100.00  161.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7300  125.0000   90.0000 61

 12 omega   20.00   82.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7300  -45.0000 -180.0000 62

 13 omega   40.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7300  -61.0000  -30.0000 73

 14 omega   84.00  154.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7300   45.0000   90.0000 70

 15 omega   27.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7300  -94.0000 -180.0000 66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0083022000
_diffrn_orient_matrix_UB_12      -0.1234022000
_diffrn_orient_matrix_UB_13      0.0071955000
_diffrn_orient_matrix_UB_21      0.0553752000
_diffrn_orient_matrix_UB_22      -0.0120748000
_diffrn_orient_matrix_UB_23      0.0845288000
_diffrn_orient_matrix_UB_31      -0.2012094000
_diffrn_orient_matrix_UB_32      0.0123751000
_diffrn_orient_matrix_UB_33      0.0277900000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_unetI/netI     0.0876
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9743
_diffrn_reflns_theta_full        63.00
_diffrn_reflns_theta_max         63.00
_diffrn_reflns_theta_min         3.58
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.152
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0948
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1738P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2378
_refine_ls_wR_factor_ref         0.2827
_reflns_number_gt                3403
_reflns_number_total             5172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            J-Mater-Chem-C-2017-5-1308.cif
_cod_data_source_block           exp_6100
_cod_database_code               7235170
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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:
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C12(H12), C15(H15), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C)
;