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#$Date: 2017-10-13 08:28:26 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201972 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/35/2103566.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2103566
loop_
_publ_author_name
'In, Yasuko'
'Fujii, Mayumi'
'Sasada, Yasuhiro'
'Ishida, Toshimasa'
_publ_section_title
;
 Structural studies on C-amidated amino acids and peptides: structures
 of hydrochloride salts of C-amidated Ile, Val, Thr, Ser, Met, Trp, Gln
 and Arg, and comparison with their C-unamidated counterparts
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              72
_journal_page_last               81
_journal_paper_doi               10.1107/S0108768100013975
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C5 H13 N2 O S +,Cl -'
_chemical_formula_sum            'C5 H13 Cl N2 O S'
_chemical_formula_weight         184.68
_chemical_name_systematic
;
 ?
;
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.591(3)
_cell_length_b                   5.029(3)
_cell_length_c                   11.786(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.48
_cell_measurement_theta_min      .3
_cell_volume                     447.0(4)
_computing_cell_refinement       'MSC/AFC (Molecular Structure Corp. 1991)'
_computing_data_collection       'MSC/AFC (Molecular Structure Corp. 1991)'
_computing_data_reduction        'MSC/AFC (Molecular Structure Corp. 1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .968
_diffrn_measured_fraction_theta_max .968
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  .0227
_diffrn_reflns_av_sigmaI/netI    .0235
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            907
_diffrn_reflns_theta_full        67.48
_diffrn_reflns_theta_max         67.48
_diffrn_reflns_theta_min         3.77
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.511
_exptl_absorpt_correction_T_max  .759
_exptl_absorpt_correction_T_min  .697
_exptl_absorpt_correction_type   '\y-scan (North, et al., 1990)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             196
_exptl_crystal_size_max          .7
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .05
_refine_diff_density_max         .568
_refine_diff_density_min         -.521
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   .01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.439
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.439
_refine_ls_R_factor_all          .0637
_refine_ls_R_factor_gt           .0592
_refine_ls_shift/su_max          .249
_refine_ls_shift/su_mean         .050
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[ω²(Fo²)+(0.1P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1634
_reflns_number_gt                811
_reflns_number_total             864
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            oa0030.cif
_cod_data_source_block           metNH2
_cod_original_sg_symbol_Hall     'P 2y1'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2103566
_cod_database_fobs_code          2103566
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Cl .51904(16) .4730 .64719(12) .0384(5) Uani d . 1 Cl
S4 .8109(2) .4047(5) .97871(12) .0431(5) Uani d . 1 S
N1 .7346(6) .4648(12) 1.4153(3) .0291(10) Uani d . 1 N
H1A .6803 .3142 1.4073 .035 Uiso d R 1 H
H1B .6930 .6258 1.4089 .035 Uiso d R 1 H
H1C .7753 .4624 1.4898 .035 Uiso d R 1 H
C1 .8676(7) .4039(13) 1.3348(4) .0292(12) Uani d . 1 C
H1 .9039 .2172 1.3427 .035 Uiso calc R 1 H
C1' 1.0272(8) .5838(14) 1.3652(5) .0300(13) Uani d . 1 C
O1' 1.0093(5) .8075(10) 1.4009(4) .0355(11) Uani d . 1 O
N2 1.1836(6) .4804(14) 1.3470(5) .0425(13) Uani d . 1 N
H2NA 1.2583 .5565 1.3601 .051 Uiso d R 1 H
H2NB 1.2061 .2906 1.3373 .051 Uiso d R 1 H
C2 .7816(6) .4573(14) 1.2116(4) .0320(12) Uani d . 1 C
H2A .6671 .3701 1.1996 .038 Uiso calc R 1 H
H2B .7630 .6469 1.2007 .038 Uiso calc R 1 H
C3 .9003(8) .3536(19) 1.1248(5) .0468(19) Uani d . 1 C
H3A .9197 .1647 1.1375 .056 Uiso calc R 1 H
H3B 1.0145 .4413 1.1380 .056 Uiso calc R 1 H
C5 .6515(10) .1451(19) .9597(7) .056(2) Uani d . 1 C
H5A .5928 .1508 .8832 .084 Uiso calc R 1 H
H5B .5658 .1676 1.0129 .084 Uiso calc R 1 H
H5C .7097 -.0234 .9727 .084 Uiso calc R 1 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cl .0321(7) .0372(8) .0472(8) .0020(6) .0097(5) .0016(7)
S4 .0492(9) .0507(12) .0317(8) -.0083(7) .0154(6) -.0003(7)
N1 .028(2) .031(2) .029(2) -.002(2) .0063(15) .002(2)
C1 .028(2) .029(3) .031(3) -.001(2) .007(2) -.002(3)
C1' .026(3) .035(3) .028(3) -.002(3) .000(2) .002(3)
O1' .0278(19) .032(3) .046(2) -.0023(18) .0012(17) -.010(2)
N2 .023(2) .039(3) .066(3) .000(2) .007(2) -.013(3)
C2 .030(2) .038(3) .029(2) -.005(3) .007(2) -.001(3)
C3 .037(3) .070(5) .035(3) .000(3) .011(2) -.010(3)
C5 .049(4) .060(5) .060(5) -.011(4) .011(3) -.014(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0492 .0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0311 .0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S .3331 .5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .3639 .7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C5 S4 C3 101.2(4)
N1 C1 C1' 107.8(5)
N1 C1 C2 108.5(4)
C1' C1 C2 111.0(5)
O1' C1' N2 123.5(6)
O1' C1' C1 121.0(6)
N2 C1' C1 115.4(6)
C3 C2 C1 110.5(5)
C2 C3 S4 113.9(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S4 C5 1.777(8)
S4 C3 1.797(6)
N1 C1 1.494(6)
C1 C1' 1.522(8)
C1 C2 1.547(7)
C1' O1' 1.214(8)
C1' N2 1.335(8)
C2 C3 1.529(8)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 17966343
