N-Tosylpyrrolidine Calix[4]pyrrole: Synthesis and Ion Binding Studies
Sung Kuk Kim; Dustin E. Gross; Dong-Gyu Cho; Vincent M. Lynch; Jonathan L. Sessler; Journal of Organic Chemistry 76 (2011) 1005–1012; doi:10.1021/jo101882r

data_4026040
_publ_section_title
;
 N-Tosylpyrrolidine Calix[4]pyrrole: Synthesis and Ion Binding Studies
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1005
_journal_page_last               1012
_journal_paper_doi               10.1021/jo101882r
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C64 H72 N8 O8 S4, C16 H36 N 1+, Cl 1-'
_chemical_formula_sum            'C80 H108 Cl N9 O8 S4'
_chemical_formula_weight         1487.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           109
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw -2'
_symmetry_space_group_name_H-M   'I 41 m d'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.5509(15)
_cell_length_b                   23.5509(15)
_cell_length_c                   14.5959(9)
_cell_measurement_reflns_used    6049
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     8095.5(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1141
_diffrn_reflns_av_sigmaI/netI    0.1002
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12049
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       prisms
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.21(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3746
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2084
_refine_ls_wR_factor_ref         0.2295
_reflns_number_gt                2121
_reflns_number_total             3746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo101882r_si_002.cif
_cod_data_source_block           ksk007
_cod_database_code               4026040