First Interchain Peptide Interaction Detected by ESR in Fully Synthetic, Template-Assisted, Two-Helix Bundles
Alessandra Polese; D. Joe Anderson; Glenn Millhauser; Fernando Formaggio; Marco Crisma; Fernando Marchiori; Claudio Toniolo; Journal of the American Chemical Society 121 (1999) 11071–11078; doi:10.1021/ja992079h

data_4116610
_publ_section_title
;
 First Interchain Peptide Interaction Detected by ESR in Fully Synthetic,
 Template-Assisted, Two-Helix Bundles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11071
_journal_page_last               11078
_journal_paper_doi               10.1021/ja992079h
_journal_volume                  121
_journal_year                    1999
_chemical_formula_moiety         'C38 H67 N7 O9, H2 O, H2 O'
_chemical_formula_sum            'C38 H71 N7 O11'
_chemical_formula_weight         802.02
_chemical_melting_point          547(1)
_chemical_name_systematic
; 
 Ac-TOAC-(Aib)2-TOAC-Aib-OtBu dihydrate
;
_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                68.40(10)
_cell_angle_beta                 89.10(10)
_cell_angle_gamma                82.80(10)
_cell_formula_units_Z            4
_cell_length_a                   10.435(2)
_cell_length_b                   20.878(3)
_cell_length_c                   24.207(3)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      11
_cell_volume                     4862(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Philips PW1100 diffractometer'
_diffrn_measurement_method       '\q-2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9347
_diffrn_reflns_theta_full        50.00
_diffrn_reflns_theta_max         50.00
_diffrn_reflns_theta_min         2.30
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1070
_refine_ls_number_reflns         9311
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1749
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.712
_refine_ls_shift/su_mean         0.052
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2472
_reflns_number_gt                3950
_reflns_number_total             9311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja992079h.cif
_cod_data_source_block           ctf25n
_cod_original_cell_volume        4862.1(13)
_cod_database_code               4116610