Determination of Peptide Backbone Torsion Angles Using Double-Quantum Dipolar Recoupling Solid-State NMR Spectroscopy
Manish A. Mehta; Matthew T. Eddy; Seth A. McNeill; Frank D. Mills; Joanna R. Long; Journal of the American Chemical Society 130 (2008) 2202–2212; doi:10.1021/ja074244w

data_4107430
_publ_section_title
;
 Determination of Peptide Backbone Torsion Angles Using Double-Quantum
 Dipolar Recoupling Solid-State NMR Spectroscopy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2202
_journal_page_last               2212
_journal_paper_doi               10.1021/ja074244w
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration syn
_chemical_formula_sum            'C7 H15 N3 O5'
_chemical_formula_weight         221.22
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.836(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.7750(8)
_cell_length_b                   5.3753(6)
_cell_length_c                   12.1491(13)
_cell_measurement_reflns_used    5678
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.8985
_cell_measurement_theta_min      2.687
_cell_volume                     495.06(9)
_computing_cell_refinement       'SAINT+ 6.45 (Bruker, 2003)'
_computing_data_collection       'SMART 5.630 (Bruker, 1997-2002)'
_computing_data_reduction        'SAINT+ 6.45'
_computing_molecular_graphics    'SHELXTL 6.10'
_computing_publication_material  'SHELXTL 6.10'
_computing_structure_refinement  'SHELXTL 6.10'
_computing_structure_solution    'SHELXTL 6.10 (Bruker, 2000)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5909
_diffrn_reflns_theta_full        30.48
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count \\infty
_diffrn_standards_interval_time  \\infty
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.8672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in SAINT+; Bruker, 1997-1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             236
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.160
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         1648
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+0.0437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                1622
_reflns_number_total             1648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074244w-file001.cif
_cod_data_source_block           04mz104m
_cod_database_code               4107430