A calix[2]phenol[2]pyrrole and a fused pyrrolidine-containing derivative
Kwan-Bok Jung; Sung Kuk Kim; Vincent M. Lynch; Dong-Gyu Cho; Jonathan L. Sessler; Chem.Commun. 48 (2012) 2495–; doi:10.1039/c2cc17888e

data_7107426
_publ_section_title
;
 A calix[2]phenol[2]pyrrole and a fused pyrrolidine-containing derivative
;
_journal_name_full               Chem.Commun.
_journal_page_first              2495
_journal_paper_doi               10.1039/c2cc17888e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety
;
C32 H38 N2 O2, C32 H37 N2 O2 1-, F 1-, 2 C16 H36 N 1+,
H2 O, 3 C H2 Cl2
;
_chemical_formula_sum            'C99 H155 Cl6 F N6 O5'
_chemical_formula_weight         1740.99
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 95.290(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.8044(8)
_cell_length_b                   10.3800(5)
_cell_length_c                   31.855(2)
_cell_measurement_reflns_used    18376
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.7
_cell_volume                     9813.0(8)
_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 0.968
_diffrn_measured_fraction_theta_max 0.968
_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     0.71075
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0977
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            18633
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             3768
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.995
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.366
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         10914
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.382
_refine_ls_R_factor_all          0.1623
_refine_ls_R_factor_gt           0.0831
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2553
_reflns_number_gt                5835
_reflns_number_total             10914
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc17888e.txt
_cod_data_source_block           (4)2-H
_cod_original_cell_volume        9813.1(8)
_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               7107426