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_7127131
_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         'C80 H134 N4 Si16, 2(C7 H8)'
_chemical_formula_sum            'C94 H150 N4 Si16'
_chemical_formula_weight         1785.61
_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_block_doi                 10.5517/ccdc.csd.cc25294q
_audit_creation_date             2019-07-09T12:21:44-00:00
_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                88.170(2)
_cell_angle_beta                 76.903(2)
_cell_angle_gamma                73.041(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8911(2)
_cell_length_b                   16.0352(4)
_cell_length_c                   19.2371(5)
_cell_measurement_reflns_used    10778
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      74.316
_cell_measurement_theta_min      3.779
_cell_volume                     2840.61(12)
_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     62.00 117.00   1.00    1.00    --   42.13 159.00 -18.00   55
  2  \w     63.00 118.00   1.00    1.00    --   42.13  77.00-180.00   55
  3  \w     16.00  96.00   1.00    1.00    --   42.13  57.00-180.00   80
  4  \w    -23.00  62.00   1.00    1.00    --   42.13 -38.00  30.00   85
  5  \w    -19.00  83.00   1.00    1.00    --   42.13 -99.00 -30.00  102
  6  \w     30.00  56.00   1.00    1.00    --   42.13  77.00-180.00   26
  7  \w     32.00  66.00   1.00    4.00    --  107.93 -30.00  60.00   34
  8  \w     32.00  67.00   1.00    4.00    --  107.93 -30.00   0.00   35
  9  \w     35.00  60.00   1.00    4.00    --  107.93 -45.00 -30.00   25
 10  \w     29.00  85.00   1.00    4.00    --  107.93 -94.00   0.00   56
 11  \w     74.00 117.00   1.00    4.00    --  107.93-125.00 -90.00   43
 12  \w     37.00  63.00   1.00    4.00    --  107.93 -30.00  30.00   26
 13  \w    127.00 154.00   1.00    4.00    --  107.93  61.00 150.00   27
 14  \w     35.00  61.00   1.00    4.00    --  107.93 -30.00 -30.00   26
 15  \w     72.00 102.00   1.00    4.00    --  107.93 -94.00 -60.00   30
 16  \w     82.00 153.00   1.00    4.00    --  107.93  30.00-150.00   71
 17  \w     80.00 115.00   1.00    4.00    --  107.93  61.00 150.00   35
 18  \w     57.00 110.00   1.00    4.00    --  107.93-125.00  90.00   53
 19  \w     37.00 126.00   1.00    4.00    --  107.93 -61.00-150.00   89
 20  \w     41.00  69.00   1.00    4.00    --  107.93 -30.00 150.00   28
 21  \w     32.00 145.00   1.00    4.00    --  107.93 -15.00-180.00  113
 22  \w     36.00 134.00   1.00    4.00    --  107.93 -77.00  90.00   98
;
_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      -0.0107921
_diffrn_orient_matrix_UB_12      -0.0544405
_diffrn_orient_matrix_UB_13      0.0673873
_diffrn_orient_matrix_UB_21      0.0866207
_diffrn_orient_matrix_UB_22      -0.0835996
_diffrn_orient_matrix_UB_23      -0.0458946
_diffrn_orient_matrix_UB_31      0.1426163
_diffrn_orient_matrix_UB_32      0.0122234
_diffrn_orient_matrix_UB_33      0.0110503
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20133
_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         68.994
_diffrn_reflns_theta_min         3.793
_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    2.002
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.599
_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    1.044
_exptl_crystal_description       prism
_exptl_crystal_F_000             966
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.441
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         10521
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0854P)^2^+0.7062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0
_reflns_number_gt                9007
_reflns_number_total             10521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04735j2.cif
_cod_data_source_block           a20190138_jmm214
_cod_depositor_comments
'Adding full bibliography for 7127131--7127134.cif.'
_cod_database_code               7127131