15N Chemical Shielding in Glycyl Tripeptides: Measurement by Solid-State NMR and Correlation with X-ray Structure
Chekmenev, Eduard Y.; Zhang, Qianwen; Waddell, Kevin W.; Mashuta, Mark S.; Wittebort, Richard J.; Journal of the American Chemical Society 126 (2004) 379–384; doi:10.1021/ja0370342

data_4060204
_publ_contact_author
;
 Richard Wittebort
;
_publ_contact_author_email       rjwitt01@athena.louisville.edu
_publ_contact_author_fax         '502 852-8147'
_publ_contact_author_phone       '502 852-6613'
_publ_section_title
;
 15N Chemical Shielding in Glycyl Tripeptides: Measurement by Solid-State
 NMR and Correlation with X-ray Structure
;
_journal_coden_ASTM              JACSAT
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              379
_journal_page_last               384
_journal_paper_doi               10.1021/ja0370342
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C7 H14 N3 O4, Cl'
_chemical_formula_sum            'C7 H14 Cl N3 O4'
_chemical_formula_weight         239.66
_chemical_name_common            'ala-gly-gly HCl'
_chemical_name_systematic
;
 alanyl-glycyl-glycine hydrochloride
;
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.2258(5)
_cell_length_b                   8.7007(9)
_cell_length_c                   22.970(2)
_cell_measurement_reflns_used    4816
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.50
_cell_volume                     1044.42(18)
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       \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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8593
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Sheldrick, G. M.; SADABS (1996).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_ls_abs_structure_details ad
_refine_ls_abs_structure_Flack   0.05(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.053
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.9950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.106
_refine_ls_wR_factor_ref         0.109
_reflns_number_gt                2065
_reflns_number_total             2214
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2020-10-02

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4060204