#------------------------------------------------------------------------------
#$Date: 2017-10-13 08:28:26 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201972 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/35/2103565.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_2103565
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         'C3 H9 N2 O2 +,Cl -'
_chemical_formula_sum            'C3 H9 Cl N2 O2'
_chemical_formula_weight         140.57
_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                 90.76(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.562(2)
_cell_length_b                   4.9986(18)
_cell_length_c                   8.519(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.40
_cell_measurement_theta_min      .3
_cell_volume                     321.98(18)
_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 .989
_diffrn_measured_fraction_theta_max .989
_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  .0499
_diffrn_reflns_av_sigmaI/netI    .0147
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            687
_diffrn_reflns_theta_full        67.40
_diffrn_reflns_theta_max         67.40
_diffrn_reflns_theta_min         5.19
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.639
_exptl_absorpt_correction_T_max  .793
_exptl_absorpt_correction_T_min  .464
_exptl_absorpt_correction_type   \y-scan
_exptl_absorpt_process_details   'North, et al., 1990'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             148
_exptl_crystal_size_max          .8
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .05
_refine_diff_density_max         .421
_refine_diff_density_min         -.497
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -.01(4)
_refine_ls_extinction_coef       .050(14)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.582
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.582
_refine_ls_R_factor_all          .0514
_refine_ls_R_factor_gt           .0499
_refine_ls_shift/su_max          .003
_refine_ls_shift/su_mean         .001
_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         .1619
_reflns_number_gt                626
_reflns_number_total             638
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            oa0030.cif
_cod_data_source_block           serNH2
_cod_original_cell_volume        322.00(18)
_cod_original_sg_symbol_Hall     'P 2y1'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2103565
_cod_database_fobs_code          2103565
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
Cl1 .00171(12) .6838 .78990(13) .0386(6) Uani d . 1 Cl
N1 .7562(4) .6763(11) .1141(4) .0275(9) Uani d . 1 N
H1A .8326 .5268 .1296 .033 Uiso d R 1 H
H1B .8350 .8265 .1235 .033 Uiso d R 1 H
H1C .7232 .6662 .0213 .033 Uiso d R 1 H
C1 .6193(5) .6279(9) .2351(4) .0238(11) Uani d . 1 C
H1 .5803 .4413 .2282 .029 Uiso calc R 1 H
C1' .4649(6) .8074(10) .1998(4) .0224(10) Uani d . 1 C
N2 .3120(5) .7451(10) .2644(5) .0387(12) Uani d . 1 N
H2NA .2111 .8826 .2582 .046 Uiso d R 1 H
H2NB .3481 .7023 .3709 .046 Uiso d R 1 H
O1' .4840(4) 1.0101(7) .1163(4) .0289(8) Uani d . 1 O
C2 .6940(6) .6800(14) .4002(4) .0317(10) Uani d . 1 C
H2A .6170 .5978 .4766 .038 Uiso calc R 1 H
H2B .8093 .5964 .4101 .038 Uiso calc R 1 H
O3 .7104(5) .9590(9) .4346(3) .0393(10) Uani d . 1 O
H3 .7685 .9829 .5442 .059 Uiso d 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
Cl1 .0274(7) .0285(8) .0601(8) -.0052(5) .0039(4) -.0005(5)
N1 .0257(16) .0281(19) .0288(14) .002(2) -.0005(12) -.0068(18)
C1 .0233(19) .018(3) .0302(16) .0057(16) -.0008(14) .0014(16)
C1' .0240(17) .018(2) .0255(15) -.0018(19) -.0031(13) .0010(16)
N2 .0234(18) .036(3) .057(2) .0065(18) .0055(16) .011(2)
O1' .0267(15) .0214(17) .0387(13) .0040(14) .0001(12) .0071(14)
C2 .033(2) .035(2) .0272(17) .005(3) -.0036(14) .004(2)
O3 .0399(17) .045(2) .0329(15) .0029(17) -.0013(13) -.0116(17)
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'
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
N1 C1 C1' 108.0(3)
N1 C1 C2 110.9(3)
C1' C1 C2 111.1(4)
O1' C1' N2 122.4(4)
O1' C1' C1 120.3(4)
N2 C1' C1 117.2(4)
O3 C2 C1 112.6(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C1 1.491(5)
C1 C1' 1.500(6)
C1 C2 1.531(5)
C1' O1' 1.247(6)
C1' N2 1.324(6)
C2 O3 1.430(8)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 17340254
