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_7127133
_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         'C90 H158 N4 Si18'
_chemical_formula_sum            'C90 H158 N4 Si18'
_chemical_formula_weight         1801.81
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-18T17:29:56-00:00
_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                90
_cell_angle_beta                 101.568(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   43.6057(12)
_cell_length_b                   8.5663(2)
_cell_length_c                   33.2570(9)
_cell_measurement_reflns_used    12899
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      74.392
_cell_measurement_theta_min      3.701
_cell_volume                     12170.5(6)
_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 1
_diffrn_measured_fraction_theta_max 1
_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   -111.00 -10.00   1.00    3.00    --  -42.13 -77.00  90.00  101
  2  \w     -4.00  30.00   1.00    3.00    --  -42.13  57.00 -30.00   34
  3  \w     -9.00  66.00   1.00    3.00    --   42.13 -99.00 -60.00   75
  4  \w     46.00  77.00   1.00   12.00    --  107.93 -45.00 -60.00   31
  5  \w     35.00  75.00   1.00   12.00    --  107.93 -45.00 -90.00   40
  6  \w     37.00 117.00   1.00   12.00    --  107.93-125.00 120.00   80
  7  \w     38.00  65.00   1.00   12.00    --  107.93 -45.00-120.00   27
  8  \w     35.00 114.00   1.00   12.00    --  107.93-125.00 -90.00   79
  9  \w     47.00  73.00   1.00   12.00    --  107.93 -45.00 -30.00   26
 10  \w     34.00  60.00   1.00   12.00    --  107.93 -30.00-180.00   26
 11  \w     64.00 108.00   1.00   12.00    --  107.93 -94.00 -60.00   44
 12  \w     47.00 158.00   1.00   12.00    --  107.93   0.00  60.00  111
 13  \w    -64.00  20.00   1.00    3.00    --  -42.13  38.00-120.00   84
 14  \w     72.00  98.00   1.00    3.00    --   42.13-125.00  30.00   26
 15  \w      6.00  63.00   1.00    3.00    --   42.13-125.00  60.00   57
 16  \w     41.00  72.00   1.00   12.00    --  107.93 -45.00-150.00   31
 17  \w     56.00  84.00   1.00   12.00    --  107.93 -77.00   0.00   28
 18  \w     44.00  71.00   1.00   12.00    --  107.93 -45.00   0.00   27
 19  \w     40.00  65.00   1.00   12.00    --  107.93 -45.00 120.00   25
 20  \w     56.00  98.00   1.00   12.00    --  107.93 -94.00 150.00   42
 21  \w     39.00  65.00   1.00   12.00    --  107.93 -45.00 150.00   26
 22  \w     42.00  68.00   1.00   12.00    --  107.93 -77.00 -90.00   26
 23  \w     37.00  74.00   1.00   12.00    --  107.93 -45.00  60.00   37
 24  \w    116.00 141.00   1.00   12.00    --  107.93 -77.00   0.00   25
 25  \w     92.00 118.00   1.00   12.00    --  107.93-125.00   0.00   26
 26  \w     77.00 105.00   1.00   12.00    --  107.93  77.00-180.00   28
 27  \w     45.00  74.00   1.00   12.00    --  107.93 -45.00  90.00   29
 28  \w     36.00 109.00   1.00   12.00    --  107.93   0.00   0.00   73
;
_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      0.0020231
_diffrn_orient_matrix_UB_12      0.1566461
_diffrn_orient_matrix_UB_13      0.023192
_diffrn_orient_matrix_UB_21      -0.0001569
_diffrn_orient_matrix_UB_22      -0.0879436
_diffrn_orient_matrix_UB_23      0.0403554
_diffrn_orient_matrix_UB_31      0.0359945
_diffrn_orient_matrix_UB_32      -0.0091061
_diffrn_orient_matrix_UB_33      0.0083398
_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  0.0558
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            43494
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.987
_diffrn_reflns_theta_min         3.728
_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    2.049
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.552
_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    0.983
_exptl_crystal_description       needle
_exptl_crystal_F_000             3912
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.589
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.069
_refine_diff_density_max         1.34
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         11316
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0933
_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^)+(0.1398P)^2^+42.7895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2494
_refine_ls_wR_factor_ref         0.2693
_reflns_Friedel_coverage         0
_reflns_number_gt                8597
_reflns_number_total             11316
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           a20200032_jmm213tris4
_cod_depositor_comments
'Adding full bibliography for 7127131--7127134.cif.'
_cod_database_code               7127133