An Efficient Approach to the Synthesis of Novel Pyrene-Fused Azaacenes
Feng, Xing; Iwanaga, Fumitaka; Hu, Jian-Yong; Tomiyasu, Hirotsugu; Nakano, Masahiro; Redshaw, Carl; Elsegood, Mark R. J.; Yamato, Takehiko; Organic Letters 15 (2013) 3594–; doi:10.1021/ol401438a

data_1512175
_publ_section_title
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 An Efficient Approach to the Synthesis of Novel Pyrene-Fused Azaacenes
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_journal_issue                   14
_journal_name_full               'Organic Letters'
_journal_page_first              3594
_journal_paper_doi               10.1021/ol401438a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C46 H30 N4 O2, 2(C H2 Cl2)'
_chemical_formula_sum            'C48 H34 Cl4 N4 O2'
_chemical_formula_weight         840.59
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 106.2962(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5480(6)
_cell_length_b                   18.7363(9)
_cell_length_c                   18.7916(9)
_cell_measurement_reflns_used    16566
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.45
_cell_volume                     3902.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44734
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.351
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         11841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+2.5754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1447
_reflns_number_gt                9567
_reflns_number_total             11841
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ol401438a_si_001.cif
_cod_data_source_block           ty17
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1512175