Molecular Recognition in Cyclodextrin Complexes of Amino Acid Derivatives. 1. Crystallographic Studies of β-Cyclodextrin Complexes with N-Acetyl-l-phenylalanine Methyl Ester and N-Acetyl-l-phenylalanine Amide Pseudopeptides
Joanna L. Clark; John J. Stezowski; Journal of the American Chemical Society 123 (2001) 9880–9888; doi:10.1021/ja003717v

data_4115713
_publ_section_title
;
 Molecular Recognition in Cyclodextrin Complexes of Amino Acid
 Derivatives. 1. Crystallographic Studies of \b-Cyclodextrin Complexes
 with N-Acetyl-l-phenylalanine Methyl Ester and N-Acetyl-l-phenylalanine
 Amide Pseudopeptides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9880
_journal_page_last               9888
_journal_paper_doi               10.1021/ja003717v
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C108 H217 N2 O100'
_chemical_formula_weight         3143.83
_chemical_name_common
'N-acetyl-L-phe methyl ester/Beta-Cyclodextrin'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           1
_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                103.970(10)
_cell_angle_beta                 112.890(10)
_cell_angle_gamma                98.790(10)
_cell_formula_units_Z            1
_cell_length_a                   18.129(2)
_cell_length_b                   15.411(2)
_cell_length_c                   15.585(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3741.5(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Syntex autodiffractometer'
_diffrn_measurement_method       omega
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13775
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.9
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(12)
_refine_ls_extinction_coef       0.0139(17)
_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   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1644
_refine_ls_number_reflns         13217
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          2.555
_refine_ls_shift/su_mean         0.047
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1717P)^2^+0.9308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2145
_refine_ls_wR_factor_ref         0.2370
_reflns_number_gt                10224
_reflns_number_total             13217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja003717v_1.cif
_cod_data_source_block           s091rm
_cod_original_cell_volume        3741.5(8)
_cod_database_code               4115713