Polyfunctional Recognition of Pyridinedicarboxylate Anions with Macrocyclic Polyamine Receptors Containing Heteroaromatic Groups
Carla Bazzicalupi; Andrea Bencini; Antonio Bianchi; Claudia Borri; Andrea Danesi; Enrique García-España; Claudia Giorgi; Barbara Valtancoli; Journal of Organic Chemistry 73 (2008) 8286–8295; doi:10.1021/jo801366w

data_4023794
_publ_section_title
;
 Polyfunctional Recognition of Pyridinedicarboxylate Anions with
 Macrocyclic Polyamine Receptors Containing Heteroaromatic Groups
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8286
_journal_page_last               8295
_journal_paper_doi               10.1021/jo801366w
_journal_volume                  73
_journal_year                    2008
_chemical_formula_sum            'C86 H120 N22 O35'
_chemical_formula_weight         2022.04
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.943(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.406(2)
_cell_length_b                   30.106(3)
_cell_length_c                   21.455(2)
_cell_measurement_temperature    298
_cell_volume                     9770.2(18)
_computing_cell_refinement       'Crysalis CCD - Oxford diffraction'
_computing_data_collection       'Crysalis CCD - Oxford diffraction'
_computing_data_reduction        'Crysalis CCD - Oxford diffraction'
_computing_molecular_graphics
;
ORTEP3 Ver. 1.01\b (Farrugia, 1997) - Mercury 2001-2007
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla 2005)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 8.1241
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur CCD'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.1890
_diffrn_reflns_av_sigmaI/netI    0.2873
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46263
_diffrn_reflns_theta_full        50.43
_diffrn_reflns_theta_max         50.43
_diffrn_reflns_theta_min         4.39
_diffrn_standards_interval_count infinity
_diffrn_standards_interval_time  infinity
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.2 (release 07-07-2006 CrysAlis171 .NET)
(compiled Jul 10 2006,00:11:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4280
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.795
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1299
_refine_ls_number_reflns         10175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.795
_refine_ls_R_factor_all          0.2429
_refine_ls_R_factor_gt           0.0808
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1911
_refine_ls_wR_factor_ref         0.2533
_reflns_number_gt                2960
_reflns_number_total             10175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo801366w_si_002.cif
_cod_data_source_block           L.4H2(2,6-pdc).H2O.0.5EtOH
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4023794