Bis(azafulvene) as a Versatile Building Block for Giant Cyclopolypyrroles: X-ray Crystal Structure of [64]Hexadecaphyrin(1.0.1.0.1.0.1.0.1.0.1.0.1.0.1.0)
Jun-ichiro Setsune; Satoshi Maeda; Journal of the American Chemical Society 122 (2000) 12405–12406; doi:10.1021/ja005588o

data_4116268
_publ_section_title
;
 Bis(azafulvene) as a Versatile Building Block for Giant
 Cyclopolypyrroles: X-ray Crystal Structure of
 [64]Hexadecaphyrin(1.0.1.0.1.0.1.0.1.0.1.0.1.0.1.0)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12405
_journal_page_last               12406
_journal_paper_doi               10.1021/ja005588o
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C184 H208 N16'
_chemical_formula_weight         2643.66
_chemical_name_systematic
; 
2,3,7,8,11,12,16,17,20,21,25,26,29,30,34,35,38,39,43,44,47,48,52,53,56,57,
61,62,65,66,70,71-dotriacontaethyl-5,14,23,32,41,50,59,68-
octaphenyl-[64]hexadecaphyrin-(1.0.1.0.1.0.1.0.1.0.1.0.1.0.1.0)  
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.085(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.611(3)
_cell_length_b                   14.3764(14)
_cell_length_c                   34.408(4)
_cell_measurement_temperature    293(2)
_cell_volume                     17077(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.877
_diffrn_measured_fraction_theta_max 0.877
_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  0.1135
_diffrn_reflns_av_sigmaI/netI    0.1372
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            45557
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5696
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         17212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.2453
_refine_ls_R_factor_gt           0.0968
_refine_ls_shift/su_max          1.296
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1647P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2442
_refine_ls_wR_factor_ref         0.3280
_reflns_number_gt                5816
_reflns_number_total             17212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja005588o_s2.cif
_cod_data_source_block           p16p
_cod_database_code               4116268