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_4026039
_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, 4 C3 H7 N O, 1/2 C H2 Cl2'
_chemical_formula_sum            'C76.5 H101 Cl N12 O12 S4'
_chemical_formula_weight         1544.38
_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                105.0390(10)
_cell_angle_beta                 90.9620(10)
_cell_angle_gamma                107.6010(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4296(6)
_cell_length_b                   12.6286(6)
_cell_length_c                   15.0391(9)
_cell_measurement_reflns_used    6881
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1987.52(18)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f and \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  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15170
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.581
_exptl_crystal_description       plates
_exptl_crystal_F_000             1642
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.0050(11)
_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   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         8976
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.2810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1341
_reflns_number_gt                5979
_reflns_number_total             8976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo101882r_si_001.cif
_cod_data_source_block           ksk001
_cod_original_formula_sum        'C76.50 H101 Cl N12 O12 S4'
_cod_database_code               4026039