The Origin of Selectivity in the Complexation of N-Methyl Amino Acids by Tetraphosphonate Cavitands.
Pinalli, Roberta; Brancatelli, Giovanna; Pedrini, Alessandro; Menozzi, Daniela; Hernández, Daniel; Ballester, Pablo; Geremia, Silvano; Dalcanale, Enrico; Journal of the American Chemical Society 138 (2016) 8569–8580; doi:10.1021/jacs.6b04372

data_4130533
_publ_section_title
;
 The Origin of Selectivity in the Complexation of N-Methyl Amino Acids by
 Tetraphosphonate Cavitands.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8569
_journal_page_last               8580
_journal_paper_doi               10.1021/jacs.6b04372
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C92 H108.9 Cl2 F18.9 N2 O33.8 P8'
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_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-07T21:16:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                67.422(3)
_cell_angle_beta                 71.903(2)
_cell_angle_gamma                82.706(2)
_cell_formula_units_Z            1
_cell_length_a                   13.1740(10)
_cell_length_b                   14.676(2)
_cell_length_c                   16.9650(10)
_cell_measurement_reflns_used    26832
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.541
_cell_measurement_theta_min      2.172
_cell_measurement_wavelength     0.7
_cell_volume                     2878.7(5)
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_molecular_graphics    Pymol
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
'SIR2011, updated version of SIR2008 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Elettra Synchrotron, Trieste (Italy)'
_diffrn_radiation_wavelength     0.7
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.889
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_number            26832
_diffrn_reflns_point_group_measured_fraction_full 0.834
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         29.541
_diffrn_reflns_theta_min         2.172
_exptl_absorpt_coefficient_mu    0.259
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_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.42
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             1269
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.195
_refine_diff_density_min         -1.372
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 11219 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(18)
_refine_ls_extinction_coef       0.0146(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1573
_refine_ls_number_reflns         26832
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1604P)^2^+1.5662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2161
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    0.779
_reflns_Friedel_fraction_max     0.738
_reflns_number_gt                25748
_reflns_number_total             26832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04372_si_014.cif
_cod_data_source_block           Tiiii_N_Me_Lys
_cod_original_formula_sum        'C92 H108.90 Cl2 F18.90 N2 O33.80 P8'
_cod_database_code               4130533
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              69523
_shelx_hkl_checksum              68093