Charge Transport Modulation in Pseudorotaxane 1D Stacks of Acene and Azaacene Derivatives
Gozálvez, Cristian; Zafra, José L.; Saeki, Akinori; Melle-Franco, Manuel; Casado Cordón, Juan; Mateo-Alonso, Aurelio; Chemical Science  (2019) –; doi:10.1039/C8SC04845B

data_1550426
_publ_section_title
;
 Charge Transport Modulation in Pseudorotaxane 1D Stacks of Acene and
 Azaacene Derivatives
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04845B
_journal_year                    2019
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C46 H34 N6 O4, C12 H8 N2 O2, 4(C2 H2 Cl4)'
_chemical_formula_sum            'C66 H50 Cl16 N8 O6'
_chemical_formula_weight         1618.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-22T13:15:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-07-29 deposited with the CCDC.
2019-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                94.092(2)
_cell_angle_beta                 92.8740(19)
_cell_angle_gamma                92.603(2)
_cell_formula_units_Z            4
_cell_length_a                   10.5616(3)
_cell_length_b                   23.6815(7)
_cell_length_c                   27.6022(5)
_cell_measurement_reflns_used    12739
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.857
_cell_measurement_theta_min      3.587
_cell_measurement_wavelength     1.54184
_cell_volume                     6869.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2012
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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    -64.00  31.00   1.00    3.00    --  -41.33  57.00   0.00   95
  2  \w   -109.00 -16.00   1.00    3.00    --  -41.33 -57.00-150.00   93
  3  \w   -116.00 -88.00   1.00    3.00    --  -41.33 -99.00   0.00   28
  4  \w      4.00  98.00   1.00    3.00    --   41.33-125.00-180.00   94
  5  \w    -78.00 -45.00   1.00   12.00    --  -83.00   0.00-150.00   33
  6  \w    -66.00 -12.00   1.00   12.00    --  -83.00  45.00  90.00   54
  7  \w    -21.00   5.00   1.00   12.00    --  -83.00   0.00-150.00   26
  8  \w    -33.00  -5.00   1.00   12.00    --  -83.00  30.00 120.00   28
  9  \w     36.00  77.00   1.00   12.00    --  108.36 -45.00 -60.00   41
 10  \w     30.00  60.00   1.00   12.00    --  108.36 -30.00-150.00   30
 11  \w     41.00  67.00   1.00   12.00    --  108.36 -45.00 120.00   26
 12  \w     46.00  85.00   1.00   12.00    --  108.36 -94.00 150.00   39
 13  \w     28.00 109.00   1.00   12.00    --  108.36 -94.00 -30.00   81
 14  \w     26.00 138.00   1.00   12.00    --  108.36   0.00  60.00  112
 15  \w     24.00 109.00   1.00   12.00    --  108.36 -94.00  60.00   85
 16  \w     61.00  88.00   1.00   12.00    --  108.36 -61.00 -30.00   27
 17  \w     45.00  99.00   1.00   12.00    --  108.36-125.00 -60.00   54
 18  \w     45.00  77.00   1.00   12.00    --  108.36 -45.00  60.00   32
 19  \w     83.00 109.00   1.00   12.00    --  108.36 -94.00-120.00   26
 20  \w     91.00 151.00   1.00   12.00    --  108.36  45.00  90.00   60
 21  \w    121.00 158.00   1.00   12.00    --  108.36  61.00  30.00   37
 22  \w    109.00 136.00   1.00   12.00    --  108.36 -61.00 -30.00   27
 23  \w     33.00  61.00   1.00   12.00    --  108.36 -30.00  90.00   28
 24  \w     33.00 122.00   1.00   12.00    --  108.36-125.00-120.00   89
 25  \w     40.00  72.00   1.00   12.00    --  108.36 -45.00-120.00   32
 26  \w     25.00  66.00   1.00   12.00    --  108.36 -94.00-120.00   41
;
_diffrn_measurement_device       'four-circle \k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1368704
_diffrn_orient_matrix_UB_12      0.0198501
_diffrn_orient_matrix_UB_13      0.0003892
_diffrn_orient_matrix_UB_21      -0.0509126
_diffrn_orient_matrix_UB_22      -0.0621316
_diffrn_orient_matrix_UB_23      -0.0014349
_diffrn_orient_matrix_UB_31      0.0074831
_diffrn_orient_matrix_UB_32      0.0030921
_diffrn_orient_matrix_UB_33      0.0560165
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova( Cu) X-ray micro-source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.1033
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53530
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.996
_diffrn_reflns_theta_min         3.6
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.346
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.206
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.439
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.526
_refine_diff_density_min         -2.487
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1831
_refine_ls_number_reflns         25968
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.1021
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1418P)^2^+29.1338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2662
_refine_ls_wR_factor_ref         0.3016
_reflns_number_gt                17707
_reflns_number_total             25968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04845b2.cif
_cod_data_source_block           a20170101_cgm3016a1
_cod_database_code               1550426