Twisted pyrene-fused azaacenes
Sandeep More; Sunil Choudhary; Alexander Higelin; Ingo Krossing; Manuel Melle-Franco; Aurelio Mateo-Alonso; Chem.Commun. 50 (2014) 1976–; doi:10.1039/c3cc48742c

data_7111950
_publ_section_title
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 Twisted pyrene-fused azaacenes
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_journal_name_full               Chem.Commun.
_journal_page_first              1976
_journal_paper_doi               10.1039/c3cc48742c
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         '(C112 H170 N4 Si6)'
_chemical_formula_sum            'C112 H170 N4 Si6'
_chemical_formula_weight         1741.06
_space_group_IT_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.745(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7047(3)
_cell_length_b                   22.2249(7)
_cell_length_c                   28.1465(9)
_cell_measurement_reflns_used    9382
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.3031
_cell_measurement_theta_min      2.3448
_cell_volume                     5382.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.867
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_sigmaI/netI    0.1335
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57575
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.7409
_exptl_absorpt_correction_T_min  0.7002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2008/1 (Bruker,2008) was used for absorption correction.
 R(int) was 0.1374 before and 0.0723 after correction.
 The Ratio of minimum to maximum transmission is 0.440766550523.
 The \l/2 correction factor is 0.0015
;
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         8262
_refine_ls_number_restraints     439
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1344
_reflns_number_gt                4794
_reflns_number_total             8262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc48742c.txt
_cod_data_source_block           SPM336_2
_cod_database_code               7111950