Conformational Analysis of Furanoid ε-Sugar Amino Acid Containing Cyclic Peptides by NMR Spectroscopy, Molecular Dynamics Simulation, and X-ray Crystallography: Evidence for a Novel Turn Structure
Renate M. van Well; Luciana Marinelli; Cornelis Altona; Kees Erkelens; Gregg Siegal; Mark van Raaij; Antonio L. Llamas-Saiz; Horst Kessler; Ettore Novellino; Antonio Lavecchia; Jacques H. van Boom; Mark Overhand; Journal of the American Chemical Society 125 (2003) 10822–10829; doi:10.1021/ja035461+

data_4114136
_publ_section_title
;
 Conformational Analysis of Furanoid \e-Sugar Amino Acid Containing Cyclic
 Peptides by NMR Spectroscopy, Molecular Dynamics Simulation, and X-ray
 Crystallography: Evidence for a Novel Turn Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10822
_journal_page_last               10829
_journal_paper_doi               10.1021/ja035461+
_journal_volume                  125
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C26 H36 N4 O10), 7(H2 O)'
_chemical_formula_sum            'C26 H43 N4 O13.5'
_chemical_formula_weight         627.64
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-08-14T18:17:59-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.194(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.578(6)
_cell_length_b                   8.438(3)
_cell_length_c                   18.997(7)
_cell_measurement_reflns_used    1739
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      2.64
_cell_measurement_wavelength     0.71073
_cell_volume                     2978.0(18)
_computing_cell_refinement       'SAINT (Bruker AXS)'
_computing_data_collection       'SMART (Bruker AXS)'
_computing_data_reduction        'SAINT (Bruker AXS), SORTAV (Blessing, 1987)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SnB 2.2 (Weeks & Miller, 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.1096
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            29861
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        28.3
_diffrn_reflns_theta_max         28.3
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.9846
_exptl_absorpt_correction_T_min  0.5712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       needle
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          1.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.76
_refine_diff_density_rms         0.215
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_coef       0.227(14)
_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   1.386
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         13595
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.411
_refine_ls_R_factor_all          0.1664
_refine_ls_R_factor_gt           0.1433
_refine_ls_shift/su_max          3.971
_refine_ls_shift/su_mean         0.173
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3781
_refine_ls_wR_factor_ref         0.3947
_reflns_number_gt                8578
_reflns_number_total             13595
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0354612Bsi20030423_032114.cif
_cod_data_source_block           rwell1n
_cod_original_cell_volume        2977.9(18)
_cod_database_code               4114136