Expanded Hexapyrrolohexaazacoronenes. Near-Infrared Absorbing Chromophores with Interrupted Peripheral Conjugation.
Gońka, Elżbieta; Chmielewski, Piotr J.; Lis, Tadeusz; Stępień, Marcin; Journal of the American Chemical Society  (2014) 141110133001000–; doi:10.1021/ja508963v

data_4122937
_publ_section_title
;
 Expanded Hexapyrrolohexaazacoronenes. Near-Infrared Absorbing
 Chromophores with Interrupted Peripheral Conjugation.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141110133001000
_journal_paper_doi               10.1021/ja508963v
_journal_year                    2014
_chemical_formula_moiety         'C157 H161 N7 O14'
_chemical_formula_sum            'C157 H161 N7 O14'
_chemical_formula_weight         2369.92
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90.33(5)
_cell_angle_beta                 108.89(5)
_cell_angle_gamma                117.02(5)
_cell_formula_units_Z            2
_cell_length_a                   18.804(8)
_cell_length_b                   20.072(9)
_cell_length_c                   20.265(9)
_cell_measurement_reflns_used    3055
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      2
_cell_volume                     6340(6)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Xcalibur PX with Onyx CCD detector'
_diffrn_measurement_method       w/
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.1283
_diffrn_reflns_av_unetI/netI     0.2857
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58348
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         79.203
_diffrn_reflns_theta_min         2.343
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5
Analytical numeric absorption correction using a
multifaceted crystal model based on expressions
derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            light-gold
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.34
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1380
_refine_ls_number_reflns         25217
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.3380
_refine_ls_R_factor_gt           0.1189
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0220P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4257
_reflns_number_total             25217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508963v_si_002.cif
_cod_data_source_block           GONK12BA
_cod_database_code               4122937
_shelx_estimated_absorpt_t_min   0.845
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           2013-2
_shelx_res_checksum              2128