Selective Amine Recognition Driven by Host-Guest Proton Transfer and Salt Bridge Formation
Calogero Capici; Giuseppe Gattuso; Anna Notti; Melchiorre F. Parisi; Sebastiano Pappalardo; Giovanna Brancatelli; Silvano Geremia; Journal of Organic Chemistry 77 (2012) 9668–9675; doi:10.1021/jo301730m

data_4027652
_publ_section_title
;
 Selective Amine Recognition Driven by Host-Guest Proton Transfer and Salt
 Bridge Formation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9668
_journal_page_last               9675
_journal_paper_doi               10.1021/jo301730m
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C81 H112 O15, C H Cl3, 1.3(C2 H3 N)'
_chemical_formula_sum            'C84.5 H117 Cl3 N1.25 O15'
_chemical_formula_weight         1496.64
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-10T13:36:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.993(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3541(2)
_cell_length_b                   28.8342(6)
_cell_length_c                   24.1281(7)
_cell_measurement_temperature    90(2)
_cell_volume                     8531.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_wavelength     0.85
_diffrn_reflns_av_unetI/netI     0.0795
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9991
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_F_000             3215
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.74
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0314(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   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     971
_refine_ls_number_reflns         9991
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0822
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1334P)^2^+16.8322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2254
_refine_ls_wR_factor_ref         0.2273
_reflns_number_gt                9445
_reflns_number_total             9991
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo301730m_si_003.cif
_cod_data_source_block           tbuco2h_(1bH)
_cod_original_formula_sum        'C84.50 H117 Cl3 N1.25 O15'
_cod_database_code               4027652