An Unusual Reverse Turn Structure Adopted by a Furanoid Sugar Amino Acid Incorporated in Gramicidin S
Gijsbert M. Grotenbreg; Mattie S. M. Timmer; Antonio L. Llamas-Saiz; Martijn Verdoes; Gijsbert A. van der Marel; Mark J. van Raaij; Herman S. Overkleeft; Mark Overhand; Journal of the American Chemical Society 126 (2004) 3444–3446; doi:10.1021/ja0397254

data_4112377
_publ_contact_author             'Llamas-Saiz, Antonio L.'
_publ_contact_author_email       raios_x@usc.es
_publ_section_title
;
 An Unusual Reverse Turn Structure Adopted by a Furanoid Sugar Amino Acid
 Incorporated in Gramicidin S
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3444
_journal_page_last               3446
_journal_paper_doi               10.1021/ja0397254
_journal_volume                  126
_journal_year                    2004
_chemical_absolute_configuration rmad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C52 H85 N11 O12'
_chemical_formula_sum            'C52 H85 N11 O12'
_chemical_formula_weight         1149.64
_chemical_name_common            gramsd
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           168
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      168
_symmetry_space_group_name_Hall  'P 6'
_symmetry_space_group_name_H-M   'P 6'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2003-07-03T13:00:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   31.3930(4)
_cell_length_b                   31.3930(4)
_cell_length_c                   12.7243(2)
_cell_measurement_reflns_used    3940
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      50.436
_cell_measurement_theta_min      1.473
_cell_measurement_wavelength     1.54184
_cell_volume                     10860.0(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       '135mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD2000
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.00306
_diffrn_orient_matrix_UB_12      -0.0307017
_diffrn_orient_matrix_UB_13      0.0308821
_diffrn_orient_matrix_UB_21      0.0359845
_diffrn_orient_matrix_UB_22      0.0179922
_diffrn_orient_matrix_UB_23      0.0162776
_diffrn_orient_matrix_UB_31      -0.0069768
_diffrn_orient_matrix_UB_32      0.0093063
_diffrn_orient_matrix_UB_33      0.0704109
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_av_unetI/netI     0.1038
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            49791
_diffrn_reflns_theta_full        50.32
_diffrn_reflns_theta_max         50.32
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_description       needle
_exptl_crystal_F_000             3700
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_extinction_coef       0.0021(2)
_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   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         7378
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.531
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1720P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2423
_refine_ls_wR_factor_ref         0.2590
_reflns_number_gt                6060
_reflns_number_total             7378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0397254si20031121_045424.cif
_cod_data_source_block           gsd17e21
_cod_database_code               4112377