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_4113809
_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            'C68 H91 Cl2 N7 O'
_chemical_formula_weight         1093.38
_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                99.666(2)
_cell_angle_beta                 98.104(2)
_cell_angle_gamma                104.904(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7430(4)
_cell_length_b                   11.5435(5)
_cell_length_c                   26.1232(12)
_cell_measurement_temperature    153(2)
_cell_volume                     3027.9(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0871
_diffrn_reflns_av_sigmaI/netI    0.2147
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16734
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       needle
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0022(6)
_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   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         10386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.2175
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+1.9786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1980
_reflns_number_gt                4468
_reflns_number_total             10386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja035089ysi20030310_100329.cif
_cod_data_source_block           cyclo7
_cod_database_code               4113809