Calix[4]pyrrole[2]carbazole: A New Kind of Expanded Calixpyrrole
Piotr Piątek; Vincent M. Lynch; Jonathan L. Sessler; Journal of the American Chemical Society 126 (2004) 16073–16076; doi:10.1021/ja045218q

data_4113248
_publ_section_title
;
 Calix[4]pyrrole[2]carbazole: A New Kind of Expanded Calixpyrrole
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16073
_journal_page_last               16076
_journal_paper_doi               10.1021/ja045218q
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C55 H58 N6'
_chemical_formula_weight         803.07
_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                90.708(1)
_cell_angle_beta                 95.949(1)
_cell_angle_gamma                97.278(1)
_cell_formula_units_Z            6
_cell_length_a                   12.8646(1)
_cell_length_b                   15.9762(2)
_cell_length_c                   32.8003(5)
_cell_measurement_temperature    153(2)
_cell_volume                     6648.81(14)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-scan
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.1424
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35058
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2580
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.00185(16)
_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   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1649
_refine_ls_number_reflns         23089
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1784
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+3.8974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                11451
_reflns_number_total             23089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja045218qsi20040808_012718.cif
_cod_data_source_block           carbclx
_cod_database_code               4113248