Increasing and dispersing strain in pyrene-fused azaacenes.
Mateos-Martín, Javier; Carini, Marco; Melle-Franco, Manuel; Mateo-Alonso, Aurelio; Chemical communications (Cambridge, England) 56 (2020) 11457–11460; doi:10.1039/d0cc04735j

data_7127134
_publ_section_title
;
 Increasing and dispersing strain in pyrene-fused azaacenes.
;
_journal_issue                   77
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11457
_journal_page_last               11460
_journal_paper_doi               10.1039/d0cc04735j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '2(C108 H146 N4 Si18), 2(C7 H8)'
_chemical_formula_sum            'C230 H308 N8 Si36'
_chemical_formula_weight         4196.07
_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     dual
_audit_creation_date             2019-11-27T11:03:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-04-21 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                74.547(4)
_cell_angle_beta                 79.773(4)
_cell_angle_gamma                71.053(5)
_cell_formula_units_Z            2
_cell_length_a                   22.1092(12)
_cell_length_b                   22.3180(13)
_cell_length_c                   29.0414(13)
_cell_measurement_reflns_used    6956
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.15
_cell_measurement_theta_min      3.644
_cell_volume                     12998.3(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      150.01(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 0.998
_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    -95.00 -58.00   1.00    1.00    --  -42.38 125.00-180.00   37
  2  \w     43.00  80.00   1.00    1.00    --   42.38  38.00 -60.00   37
  3  \w     17.00 119.00   1.00    1.00    --   42.38  77.00  90.00  102
  4  \w    -27.00  67.00   1.00    1.00    --   42.38 -57.00 -30.00   94
  5  \w    -27.00  67.00   1.00    1.00    --   42.38 -38.00 150.00   94
  6  \w     83.00 158.00   1.00    4.00    --  107.93  30.00-120.00   75
  7  \w     33.00  69.00   1.00    4.00    --  107.93 -30.00 120.00   36
  8  \w     84.00 147.00   1.00    4.00    --  107.93  30.00  30.00   63
  9  \w     83.00 116.00   1.00    4.00    --  107.93-125.00-150.00   33
 10  \w     32.00  69.00   1.00    4.00    --  107.93 -30.00 -90.00   37
 11  \w     34.00  67.00   1.00    4.00    --  107.93 -30.00-120.00   33
 12  \w     80.00 115.00   1.00    4.00    --  107.93-125.00  60.00   35
 13  \w     82.00 156.00   1.00    4.00    --  107.93  45.00 -90.00   74
 14  \w     35.00  85.00   1.00    4.00    --  107.93-125.00 120.00   50
 15  \w     93.00 118.00   1.00    4.00    --  107.93-125.00 -30.00   25
 16  \w     59.00  86.00   1.00    4.00    --  107.93-125.00 -30.00   27
 17  \w     35.00  69.00   1.00    4.00    --  107.93 -45.00  60.00   34
 18  \w     26.00 110.00   1.00    4.00    --  107.93 -94.00  60.00   84
 19  \w     52.00 117.00   1.00    4.00    --  107.93 -61.00  90.00   65
 20  \w     73.00 128.00   1.00    4.00    --  107.93 -61.00 -90.00   55
 21  \w     78.00 150.00   1.00    4.00    --  107.93  15.00-180.00   72
 22  \w     38.00 132.00   1.00    4.00    --  107.93 -77.00-150.00   94
;
_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      0.0408282
_diffrn_orient_matrix_UB_12      0.0403743
_diffrn_orient_matrix_UB_13      0.0074032
_diffrn_orient_matrix_UB_21      -0.0308771
_diffrn_orient_matrix_UB_22      0.0561634
_diffrn_orient_matrix_UB_23      -0.0406593
_diffrn_orient_matrix_UB_31      -0.0534953
_diffrn_orient_matrix_UB_32      0.0287085
_diffrn_orient_matrix_UB_33      0.0367635
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1015
_diffrn_reflns_av_unetI/netI     0.2073
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            95702
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.988
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            yellow
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description       plate
_exptl_crystal_F_000             4496
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.473
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.672
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2431
_refine_ls_number_reflns         48242
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.2193
_refine_ls_R_factor_gt           0.1286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3079
_refine_ls_wR_factor_ref         0.4078
_reflns_Friedel_coverage         0
_reflns_number_gt                21047
_reflns_number_total             48242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04735j2.cif
_cod_data_source_block           a20190139_jmm212b
_cod_depositor_comments
'Adding full bibliography for 7127131--7127134.cif.'
_cod_original_cell_volume        12998.0(10)
_cod_database_code               7127134