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_7127132
_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         'C52 H34 O4 Si2'
_chemical_formula_sum            'C52 H34 O4 Si2'
_chemical_formula_weight         778.97
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-04-29T14:11:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-04-20 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.967(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4193(9)
_cell_length_b                   15.3229(7)
_cell_length_c                   18.2720(6)
_cell_measurement_reflns_used    5581
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.288
_cell_measurement_theta_min      4.213
_cell_volume                     4027.4(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 5.2012
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.999
_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     61.00  92.00   1.00    1.00    --   42.13-125.00-180.00   31
  2  \w     14.00 104.00   1.00    1.00    --   42.13  57.00-180.00   90
  3  \w     32.00 116.00   1.00    1.00    --   42.13  38.00 -90.00   84
  4  \w     32.00  68.00   1.00    1.50    --  107.93 -30.00  60.00   36
  5  \w     32.00  69.00   1.00    1.50    --  107.93 -30.00  90.00   37
  6  \w    108.00 136.00   1.00    1.50    --  107.93  45.00-180.00   28
  7  \w     32.00  69.00   1.00    1.50    --  107.93 -30.00   0.00   37
  8  \w     34.00  66.00   1.00    1.50    --  107.93 -30.00  30.00   32
  9  \w     32.00  66.00   1.00    1.50    --  107.93 -30.00 -30.00   34
 10  \w     53.00 118.00   1.00    1.50    --  107.93-125.00-120.00   65
 11  \w     31.00  81.00   1.00    1.50    --  107.93 -94.00 -60.00   50
 12  \w     33.00  69.00   1.00    1.50    --  107.93 -30.00 120.00   36
 13  \w     55.00 112.00   1.00    1.50    --  107.93-125.00  90.00   57
 14  \w     35.00  63.00   1.00    1.50    --  107.93 -30.00-150.00   28
 15  \w     36.00  71.00   1.00    1.50    --  107.93 -45.00 -90.00   35
 16  \w      8.00 104.00   1.00    1.00    --   42.13  19.00  30.00   96
 17  \w     10.00  74.00   1.00    1.00    --   42.13-125.00 120.00   64
 18  \w     46.00  87.00   1.00    1.00    --   42.13-125.00 -30.00   41
 19  \w     36.00  95.00   1.00    1.50    --  107.93 -94.00 120.00   59
 20  \w     32.00  67.00   1.00    1.50    --  107.93 -30.00 -60.00   35
 21  \w     36.00  94.00   1.00    1.50    --  107.93 -77.00 -30.00   58
 22  \w     82.00 109.00   1.00    1.50    --  107.93 -94.00 -90.00   27
 23  \w     35.00  65.00   1.00    1.50    --  107.93 -45.00 120.00   30
 24  \w    100.00 156.00   1.00    1.50    --  107.93 125.00   0.00   56
 25  \w     95.00 145.00   1.00    1.50    --  107.93  45.00-150.00   50
 26  \w     57.00  84.00   1.00    1.50    --  107.93  15.00 -30.00   27
 27  \w     86.00 154.00   1.00    1.50    --  107.93  15.00 -30.00   68
 28  \w     69.00 116.00   1.00    1.50    --  107.93-125.00-150.00   47
 29  \w     61.00 118.00   1.00    1.50    --  107.93-125.00 -60.00   57
 30  \w    114.00 141.00   1.00    1.50    --  107.93 -77.00 -30.00   27
 31  \w     33.00  62.00   1.00    1.50    --  107.93 -30.00-180.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0438127
_diffrn_orient_matrix_UB_12      -0.0006888
_diffrn_orient_matrix_UB_13      0.0746032
_diffrn_orient_matrix_UB_21      0.0963343
_diffrn_orient_matrix_UB_22      -0.0170231
_diffrn_orient_matrix_UB_23      0.0391021
_diffrn_orient_matrix_UB_31      0.0161672
_diffrn_orient_matrix_UB_32      0.09909
_diffrn_orient_matrix_UB_33      0.0071863
_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  0.072
_diffrn_reflns_av_unetI/netI     0.1006
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33664
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.999
_diffrn_reflns_theta_min         3.769
_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    1.178
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.674
_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            orange
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       prism
_exptl_crystal_F_000             1624
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.498
_exptl_crystal_size_mid          0.332
_exptl_crystal_size_min          0.191
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         7641
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0692
_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^)+(0.1217P)^2^+1.8473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1897
_refine_ls_wR_factor_ref         0.2211
_reflns_Friedel_coverage         0
_reflns_number_gt                5190
_reflns_number_total             7641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04735j2.cif
_cod_data_source_block           a20180174_jmm187
_cod_depositor_comments
'Adding full bibliography for 7127131--7127134.cif.'
_cod_original_cell_volume        4027.5(3)
_cod_database_code               7127132