#------------------------------------------------------------------------------
#$Date: 2021-10-01 14:03:51 +0300 (Fri, 01 Oct 2021) $
#$Revision: 269432 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/30/06/2300684.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_2300684
loop_
_publ_author_name
'Jha, Kunal Kumar'
'Gruza, Barbara'
'Chodkiewicz, Michał Leszek'
'Jelsch, Christian'
'Dominiak, Paulina Maria'
_publ_section_title
;
 Refinements on electron diffraction data of β-glycine in MoPro: a quest
 for an improved structure model
;
_journal_coeditor_code           TE5073SUP1
_journal_issue                   4
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              1234
_journal_page_last               1243
_journal_paper_doi               10.1107/S160057672100580X
_journal_volume                  54
_journal_year                    2021
_chemical_formula_moiety         'C2 H5 N O2'
_chemical_formula_sum            'C2 H5 N O2'
_chemical_formula_weight         75.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_audit_contact_author_name
;
;
_audit_creation_date             2020-11-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                90
_cell_angle_beta                 112.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.3110(11)
_cell_length_b                   6.4540(13)
_cell_length_c                   5.6940(11)
_cell_measurement_temperature    103.15
_cell_volume                     179.84(7)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      103.15
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'transmission electron microscope'
_diffrn_measurement_method       'Phi scan'
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02508
_diffrn_reflns_av_R_equivalents  0.0
_diffrn_reflns_av_unetI/netI     0.2272
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_number            859
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        0.862
_diffrn_reflns_theta_max         0.957
_diffrn_reflns_theta_min         0.137
_diffrn_source
'JEOL JEM-2100 LaB6 transmission electron microscope'
_exptl_absorpt_coefficient_mu    0.119
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             28
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.36
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 179 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.410
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         859
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.364
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.1333
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2674
_refine_ls_wR_factor_ref         0.2733
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                736
_reflns_number_total             859
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            te5073sup1.cif
_cod_data_source_block           IAM_Shelx
_cod_database_code               2300684
_shelx_shelxl_version_number     2016/4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.001 within 2A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.003 and
sigma for terminal atoms of 0.003
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
;
_shelx_res_file
;
TITL Beta glycine in P2(1) solved Shelxt
 beta_gly.res created by SHELXL-2016/4 at 10:57:03 on 27-Nov-2020
REM ------ Electron scattering factors ------
CELL 0.02508 5.311 6.454 5.694 90 112.863 90
ZERR 2 0.0011 0.0013 0.0011 0 0.03 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC  C 0.136 0.373 0.548 3.281 1.227 13.046 0.597 41.02 0 0.001 0.001 =
 11.182 0.77 12.011
SFAC  H 0.037 0.561 0.127 3.791 0.236 13.556 0.129 37.723 0 0.001 0.001 =
 0.623 0.32 1.008
SFAC  N 0.137 0.329 0.534 2.673 1.086 10.317 0.455 32.763 0 0.001 0.001 =
 18.982 0.75 14.007
SFAC  O 0.143 0.305 0.51 2.268 0.937 8.262 0.392 25.665 0 0.001 0.001 =
 31.371 0.73 15.999
UNIT 4 10 2 4

SIMU 0.001 0.001 2
RIGU 0.002 0.002
ISOR 0.003 0.003

L.S. 20
PLAN  2
TEMP -170
CONF
LIST 4
BOND $H
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\beta_Gly.hkl">
REM </olex2.extras>

WGHT    0.000000
FVAR      63.45825
N1    3    0.852132    0.434862    0.235494    11.00000    0.00869    0.01250 =
         0.01345   -0.00119    0.00642    0.00037
H1A   2    0.843325    0.468138    0.022321    11.00000    0.00982
H1B   2    1.042713    0.500099    0.380362    11.00000    0.05911
H1C   2    0.855115    0.247476    0.276184    11.00000    0.02810
C1    1    0.616088    0.547250    0.273519    11.00000    0.00866    0.01259 =
         0.01382   -0.00076    0.00633    0.00016
H1D   2    0.624154    0.718820    0.214894    11.00000    0.03142
H1E   2    0.385794    0.472445    0.105650    11.00000    0.05139
C2    1    0.636340    0.536674    0.558686    11.00000    0.00766    0.01308 =
         0.01393   -0.00050    0.00670    0.00032
O1    4    0.880440    0.509168    0.742524    11.00000    0.00706    0.01433 =
         0.01377    0.00056    0.00634   -0.00030
O2    4    0.410531    0.565259    0.599982    11.00000    0.00759    0.01296 =
         0.01477   -0.00150    0.00681    0.00095
HKLF 4




REM  Beta glycine in P2(1) solved Shelxt
REM R1 =  0.1333 for     736 Fo > 4sig(Fo)  and  0.1410 for all     859 data
REM     66 parameters refined using     79 restraints

END

WGHT      0.1534      0.0000

REM Highest difference peak  0.195,  deepest hole -0.268,  1-sigma level  0.067
Q1    1   1.2094  0.3587  0.3129  11.00000  0.05    0.19
Q2    1   0.7189  0.9133  0.1960  11.00000  0.05    0.16
;
_shelx_res_checksum              12777
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.8521(14) 0.4349(9) 0.2355(14) 0.0109(10) Uani 1 1 d . U . . .
H1A H 0.843(7) 0.468(4) 0.022(7) 0.010(6) Uiso 1 1 d . . . . .
H1B H 1.043(16) 0.500(11) 0.380(16) 0.059(17) Uiso 1 1 d . . . . .
H1C H 0.855(10) 0.247(7) 0.276(10) 0.028(8) Uiso 1 1 d . . . . .
C1 C 0.6161(14) 0.5472(9) 0.2735(15) 0.0111(10) Uani 1 1 d . U . . .
H1D H 0.624(10) 0.719(7) 0.215(11) 0.031(10) Uiso 1 1 d . . . . .
H1E H 0.386(14) 0.472(9) 0.106(14) 0.051(14) Uiso 1 1 d . . . . .
C2 C 0.6363(14) 0.5367(9) 0.5587(16) 0.0108(9) Uani 1 1 d . U . . .
O1 O 0.8804(12) 0.5092(8) 0.7425(12) 0.0110(10) Uani 1 1 d . U . . .
O2 O 0.4105(11) 0.5653(8) 0.6000(13) 0.0110(10) Uani 1 1 d . U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0087(17) 0.0125(16) 0.0135(18) -0.0012(14) 0.0064(14) 0.0004(14)
C1 0.0087(15) 0.0126(14) 0.0138(16) -0.0008(13) 0.0063(12) 0.0002(12)
C2 0.0077(14) 0.0131(13) 0.0139(15) -0.0005(11) 0.0067(11) 0.0003(11)
O1 0.0071(16) 0.0143(15) 0.0138(17) 0.0006(13) 0.0063(13) -0.0003(13)
O2 0.0076(16) 0.0130(15) 0.0148(16) -0.0015(14) 0.0068(13) 0.0009(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0010 0.0010 'Peng, L M (1999) Micron 30 625 648'
H H 0.0010 0.0010 'Peng, L M (1999) Micron 30 625 648'
N N 0.0010 0.0010 'Peng, L M (1999) Micron 30 625 648'
O O 0.0010 0.0010 'Peng, L M (1999) Micron 30 625 648'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
H1A N1 H1B 110(3) . .
H1A N1 H1C 111(3) . .
H1B N1 H1C 107(5) . .
C1 N1 H1A 109.9(16) . .
C1 N1 H1B 106(4) . .
C1 N1 H1C 113(2) . .
N1 C1 H1D 107(2) . .
N1 C1 H1E 108(2) . .
N1 C1 C2 112.9(6) . .
H1D C1 H1E 106(4) . .
C2 C1 H1D 110(3) . .
C2 C1 H1E 114(2) . .
O1 C2 C1 118.1(5) . .
O2 C2 C1 118.1(7) . .
O2 C2 O1 123.7(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 H1A 1.22(3) .
N1 H1B 1.11(9) .
N1 H1C 1.23(4) .
N1 C1 1.535(8) .
C1 H1D 1.16(5) .
C1 H1E 1.32(8) .
C1 C2 1.587(10) .
C2 O1 1.324(10) .
C2 O2 1.322(7) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
N1 C1 C2 O1 24.7(8) . . . .
N1 C1 C2 O2 -158.3(5) . . . .
