#------------------------------------------------------------------------------
#$Date: 2022-09-15 01:26:15 +0300 (Thu, 15 Sep 2022) $
#$Revision: 277847 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/02/4060205.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4060205
loop_
_publ_author_name
'Chekmenev, Eduard Y.'
'Zhang, Qianwen'
'Waddell, Kevin W.'
'Mashuta, Mark S.'
'Wittebort, Richard J.'
_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         'C9 H18 N3 O4, Cl'
_chemical_formula_sum            'C9 H18 Cl N3 O4'
_chemical_formula_weight         267.71
_chemical_name_common            'gly-gly-val HCl'
_chemical_name_systematic
;
 glycyl-glycyl-valine 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                   6.9890(8)
_cell_length_b                   8.2684(10)
_cell_length_c                   21.834(3)
_cell_measurement_reflns_used    6939
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.63
_cell_volume                     1261.8(3)
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω-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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11002
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.311
_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    1.409
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.331
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.056
_refine_ls_abs_structure_details ad
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.027
_refine_ls_R_factor_gt           0.024
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0289P)²+0.1972P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.054
_refine_ls_wR_factor_ref         0.055
_reflns_number_gt                2693
_reflns_number_total             2931
_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               4060205
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.88247(13) 0.21185(11) 0.80008(4) 0.0150(2) Uani 1 1 d . . .
O2 O 0.25346(14) 0.11938(10) 0.88398(4) 0.0150(2) Uani 1 1 d . . .
O3 O -0.02803(14) 0.57366(10) 0.82543(4) 0.01532(19) Uani 1 1 d . . .
O4 O -0.23272(15) 0.53718(12) 0.90324(4) 0.0179(2) Uani 1 1 d . . .
H4O H -0.310(3) 0.592(2) 0.8803(9) 0.035(5) Uiso 1 1 d . . .
N1 N 1.07264(17) -0.06723(14) 0.79599(6) 0.0143(2) Uani 1 1 d . . .
H1NA H 1.086(2) -0.026(2) 0.7598(9) 0.028(5) Uiso 1 1 d . . .
H1NB H 1.135(2) -0.014(2) 0.8233(8) 0.022(4) Uiso 1 1 d . . .
H1NC H 1.128(3) -0.168(2) 0.7952(9) 0.038(5) Uiso 1 1 d . . .
N2 N 0.59881(16) 0.10170(14) 0.82712(6) 0.0147(2) Uani 1 1 d . . .
H2N H 0.541(2) 0.023(2) 0.8356(7) 0.016(4) Uiso 1 1 d . . .
N3 N 0.24653(17) 0.39363(13) 0.87986(5) 0.0139(2) Uani 1 1 d . . .
H3N H 0.304(2) 0.475(2) 0.8670(7) 0.015(4) Uiso 1 1 d . . .
C1 C 0.8696(2) -0.07471(17) 0.81313(7) 0.0173(3) Uani 1 1 d . . .
H1A H 0.811(2) -0.144(2) 0.7860(8) 0.020(4) Uiso 1 1 d . . .
H1B H 0.855(3) -0.123(2) 0.8530(8) 0.030(5) Uiso 1 1 d . . .
C2 C 0.78320(19) 0.09412(15) 0.81222(6) 0.0123(3) Uani 1 1 d . . .
C3 C 0.50062(19) 0.25549(15) 0.82776(7) 0.0171(3) Uani 1 1 d . . .
H3A H 0.463(2) 0.283(2) 0.7863(8) 0.024(4) Uiso 1 1 d . . .
H3B H 0.584(2) 0.3293(18) 0.8429(7) 0.015(4) Uiso 1 1 d . . .
C4 C 0.32195(18) 0.24988(15) 0.86702(6) 0.0125(3) Uani 1 1 d . . .
C5 C 0.06865(19) 0.41304(15) 0.91271(6) 0.0138(3) Uani 1 1 d . . .
H5 H 0.011(2) 0.3051(19) 0.9167(7) 0.016(4) Uiso 1 1 d . . .
C6 C -0.06748(19) 0.51627(15) 0.87508(6) 0.0132(3) Uani 1 1 d . . .
C7 C 0.0958(2) 0.48289(18) 0.97780(6) 0.0194(3) Uani 1 1 d . . .
H7 H -0.028(2) 0.4704(17) 0.9965(6) 0.013(4) Uiso 1 1 d . . .
C8 C 0.1626(3) 0.6583(2) 0.97688(8) 0.0200(4) Uani 1 1 d . . .
H8A H 0.075(3) 0.725(2) 0.9570(8) 0.029(5) Uiso 1 1 d . . .
H8B H 0.288(3) 0.665(2) 0.9579(8) 0.033(5) Uiso 1 1 d . . .
H8C H 0.171(3) 0.696(2) 1.0193(9) 0.038(5) Uiso 1 1 d . . .
C9 C 0.2343(3) 0.3764(2) 1.01359(8) 0.0208(4) Uani 1 1 d . . .
H9A H 0.205(3) 0.263(3) 1.0120(9) 0.034(6) Uiso 1 1 d . . .
H9B H 0.367(3) 0.384(2) 0.9961(8) 0.035(5) Uiso 1 1 d . . .
H9C H 0.239(3) 0.413(2) 1.0546(10) 0.036(6) Uiso 1 1 d . . .
Cl1 Cl 0.46354(5) 0.71662(4) 0.833359(15) 0.01732(8) Uani 1 1 d . . .
