#------------------------------------------------------------------------------
#$Date: 2020-02-05 06:53:45 +0100 (Wed 05 de Feb de 2020) $
#$Revision: 247887 $
#$URL: svn://www.crystallography.net/cod/cif/2/31/11/2311103.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_2311103
loop_
_publ_author_name
'Sovago, Ioana'
'Hoser, Anna A.'
'Madsen, Anders Ø.'
_publ_section_title
;
 A combined model of electron density and lattice dynamics refined against
 elastic diffraction data. Thermodynamic properties of crystalline
 <small>L</small>-alanine
;
_journal_coeditor_code           AE5068
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section A'
_journal_page_first              32
_journal_page_last               44
_journal_paper_doi               10.1107/S205327331901355X
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C3 H7 N O2'
_chemical_formula_sum            'C3 H7 N O2'
_chemical_formula_weight         89.1
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9534(5)
_cell_length_b                   12.2772(10)
_cell_length_c                   5.7882(5)
_cell_measurement_reflns_used    5997
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      58.0
_cell_measurement_theta_min      3.3
_cell_measurement_wavelength     0.71073
_cell_volume                     423.07(6)
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Nonius X8 APEXII CCD area-detector'
_diffrn_measurement_method       'ω and φ'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.027
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5997
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         57.97
_diffrn_reflns_theta_min         3.319
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.7514
_exptl_absorpt_correction_T_min  0.6454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             192
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.184
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 2422 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.11(8)
_refine_ls_extinction_coef       0.17(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.435
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         5997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.435
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0321P)²+0.0037P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                5719
_reflns_number_total             5997
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ae5068sup1.cif
_cod_data_source_block           shelx_NoMoRe_gamma
_cod_depositor_comments
'Adding full bibliography for 2311101--2311106.cif.'
_cod_database_code               2311103
_cod_database_fobs_code          2311103
_shelx_res_file
;

    test.res created by SHELXL-2014/7

TITL lAlanine 23K
CELL  0.71073   5.9534  12.2772   5.7882   90.000   90.000   90.000
ZERR     4.00   0.0005   0.0010   0.0005    0.000    0.000    0.000
LATT  -1
SYMM  1/2 - X, - Y, 1/2 + Z
SYMM  1/2 + X, 1/2 - Y, - Z
SYMM  - X, 1/2 + Y, 1/2 - Z
SFAC  O    N    C    H
UNIT  8 4 12 28
MERG   2
OMIT     0  10   0
OMIT     0   0   6
OMIT     1   2   0
FMAP   2
PLAN   20
ACTA
BOND   $H
CONF
LIST   4
L.S.  10
TEMP  -150.15
WGHT    0.032100    0.003700
EXTI    0.168339
FVAR       2.88114
O1    1    0.727659    0.083901    0.625365    11.00000   10.01460   10.01466 =
        10.01098   10.00123    9.99834   10.00515
O2    1    0.443544    0.184364    0.761300    11.00000   10.01608   10.01631 =
        10.00716    9.99887   10.00011   10.00454
N1    2    0.649280    0.137703    0.183853    11.00000   10.01249   10.01040 =
        10.00713    9.99999   10.00031   10.00011
C1    3    0.555823    0.140903    0.600372    11.00000   10.01061   10.00870 =
        10.00667    9.99986    9.99919   10.00057
C2    3    0.469019    0.161183    0.354708    11.00000   10.01104   10.00920 =
        10.00687    9.99991    9.99916   10.00106
C3    3    0.263876    0.090937    0.303311    11.00000   10.01287   10.01807 =
        10.01149    9.99855    9.99782    9.99736
H11   4    0.699222    0.065870    0.190963    11.00000   10.02393   10.01770 =
        10.02557   10.00157   10.00276   10.00490
H12   4    0.761764    0.179371    0.206811    11.00000   10.02150   10.02436 =
        10.02017    9.99902   10.00112    9.99414
H13   4    0.594003    0.148971    0.033034    11.00000   10.02600   10.02535 =
        10.01296   10.00006    9.99873   10.00026
H21   4    0.429086    0.236860    0.343368    11.00000   10.02822   10.01574 =
        10.02188   10.00088    9.99927   10.00548
H31   4    0.202081    0.108352    0.149959    11.00000   10.03469   10.04736 =
        10.02229   10.00327    9.98686    9.99425
H32   4    0.147284    0.104888    0.414920    11.00000   10.02200   10.04389 =
        10.02972    9.99531   10.00656    9.99627
H33   4    0.300993    0.012625    0.302722    11.00000   10.03642   10.02060 =
        10.03861    9.99635    9.99715    9.99575
HKLF 4

REM R1 =  0.0291 for    5719 Fo > 4sig(Fo)  and  0.0311 for all    5997 data
REM     41 parameters refined using      0 restraints

;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
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
O1 O 0.72766(5) 0.08390(2) 0.62537(5) 0.013 Uani 1 1 d
O2 O 0.44354(5) 0.18436(2) 0.76130(5) 0.013 Uani 1 1 d
N1 N 0.64928(5) 0.13770(2) 0.18385(5) 0.010 Uani 1 1 d
C1 C 0.55582(5) 0.14090(2) 0.60037(5) 0.009 Uani 1 1 d
C2 C 0.46902(5) 0.16118(2) 0.35471(5) 0.009 Uani 1 1 d
C3 C 0.26388(7) 0.09094(4) 0.30331(7) 0.014 Uani 1 1 d
H11 H 0.699(2) 0.0659(12) 0.191(3) 0.022 Uani 1 1 d
H12 H 0.762(2) 0.1794(12) 0.207(2) 0.022 Uani 1 1 d
H13 H 0.594(2) 0.1490(11) 0.033(2) 0.021 Uani 1 1 d
H21 H 0.429(2) 0.2369(10) 0.343(3) 0.022 Uani 1 1 d
H31 H 0.202(2) 0.1084(13) 0.150(3) 0.035 Uani 1 1 d
H32 H 0.147(2) 0.1049(12) 0.415(3) 0.032 Uani 1 1 d
H33 H 0.301(3) 0.0126(13) 0.303(3) 0.032 Uani 1 1 d
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
O1 0.015 0.015 0.011 0.001 -0.002 0.005
O2 0.016 0.016 0.007 -0.001 0.000 0.005
N1 0.012 0.010 0.007 0.000 0.000 0.000
C1 0.011 0.009 0.007 0.000 -0.001 0.001
C2 0.011 0.009 0.007 0.000 -0.001 0.001
C3 0.013 0.018 0.011 -0.001 -0.002 -0.003
H11 0.024 0.018 0.026 0.002 0.003 0.005
H12 0.022 0.024 0.020 -0.001 0.001 -0.006
H13 0.026 0.025 0.013 0.000 -0.001 0.000
H21 0.028 0.016 0.022 0.001 -0.001 0.005
H31 0.035 0.047 0.022 0.003 -0.013 -0.006
H32 0.022 0.044 0.030 -0.005 0.007 -0.004
H33 0.036 0.021 0.039 -0.004 -0.003 -0.004
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C2 N1 H11 112.6(9)
C2 N1 H12 110.3(9)
H11 N1 H12 108.1(13)
C2 N1 H13 109.6(8)
H11 N1 H13 106.9(12)
H12 N1 H13 109.3(12)
O1 C1 O2 125.77(3)
O1 C1 C2 118.35(3)
O2 C1 C2 115.88(3)
N1 C2 C3 109.79(3)
N1 C2 C1 109.99(2)
C3 C2 C1 111.05(3)
N1 C2 H21 108.7(8)
C3 C2 H21 109.6(9)
C1 C2 H21 107.7(9)
C2 C3 H31 110.6(9)
C2 C3 H32 110.2(8)
H31 C3 H32 107.3(14)
C2 C3 H33 111.9(9)
H31 C3 H33 107.0(13)
H32 C3 H33 109.7(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C1 1.2479(4)
O2 C1 1.2646(4)
N1 C2 1.4876(4)
N1 H11 0.932(14)
N1 H12 0.853(14)
N1 H13 0.943(13)
C1 C2 1.5333(4)
C2 C3 1.5244(5)
C2 H21 0.961(13)
C3 H31 0.984(14)
C3 H32 0.964(15)
C3 H33 0.987(16)
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
O1 C1 C2 N1 -18.25(4)
O2 C1 C2 N1 161.88(3)
O1 C1 C2 C3 103.49(4)
O2 C1 C2 C3 -76.38(4)
