Glycopolypeptides with a Redox-Triggered Helix-to-Coil Transition
Jessica R. Kramer; Timothy J. Deming; Journal of the American Chemical Society 134 (2012) 4112–4115; doi:10.1021/ja3007484

data_4117619
_publ_section_title
;
 Glycopolypeptides with a Redox-Triggered Helix-to-Coil Transition
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4112
_journal_page_last               4115
_journal_paper_doi               10.1021/ja3007484
_journal_volume                  134
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C21 H29 N O14 S, C4 H8 O'
_chemical_formula_sum            'C25 H37 N O15 S'
_chemical_formula_weight         623.62
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.864(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.622(3)
_cell_length_b                   5.2414(14)
_cell_length_c                   22.052(6)
_cell_measurement_reflns_used    8487
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.79
_cell_measurement_theta_min      3.62
_cell_volume                     1455.6(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            19671
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         3.62
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  0.9963
_exptl_absorpt_correction_T_min  0.9145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       platelet
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         8117
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1006P)^2^+0.1701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1826
_reflns_number_gt                5858
_reflns_number_total             8117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3007484_si_002.cif
_cod_data_source_block           new
_cod_original_cell_volume        1455.5(7)
_cod_database_code               4117619