Formation and Properties of Cyclo[6]pyrrole and Cyclo[7]pyrrole
Thomas Köhler; Daniel Seidel; Vincent Lynch; Forrest O. Arp; Zhongping Ou; Karl M. Kadish; Jonathan L. Sessler; Journal of the American Chemical Society 125 (2003) 6872–6873; doi:10.1021/ja035089y

data_4113808
_publ_section_title
;
 Formation and Properties of Cyclo[6]pyrrole and Cyclo[7]pyrrole
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6872
_journal_page_last               6873
_journal_paper_doi               10.1021/ja035089y
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C52 H66 F6 N6 O4'
_chemical_formula_weight         953.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.377(2)
_cell_angle_beta                 74.543(2)
_cell_angle_gamma                89.209(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9346(4)
_cell_length_b                   11.0747(4)
_cell_length_c                   11.5478(4)
_cell_measurement_temperature    153(2)
_cell_volume                     1206.97(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9461
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'very dark'
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       'prisms and plates'
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.032(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.5418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                4118
_reflns_number_total             5381
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja035089ysi20030310_100308.cif
_cod_data_source_block           hextfa
_cod_original_cell_volume        1206.97(7)
_cod_database_code               4113808