#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:59:10 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180525 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/94/7219429.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_7219429
loop_
_publ_author_name
'Zakharov, Boris A.'
'Tumanov, Nikolay A.'
'Boldyreva, Elena V.'
_publ_section_title
;
 β-Alanine under pressure: towards understanding the nature of phase
 transitions
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2074
_journal_paper_doi               10.1039/C4CE02550D
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C3 H7 N O2'
_chemical_formula_sum            'C3 H7 N O2'
_chemical_formula_weight         89.10
_chemical_name_common            beta-Alanine
_chemical_name_systematic        '3-Aminopropanoic acid'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2014-12-10 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.32(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.2593(14)
_cell_length_b                   13.10(4)
_cell_length_c                   4.7408(10)
_cell_measurement_reflns_used    137
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.7630
_cell_measurement_theta_min      3.8880
_cell_volume                     325.7(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'FOX V. (Favre-Nicolin and R. Cerny, 2002)'
_diffrn_ambient_pressure         6200000(50000)
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.239
_diffrn_measured_fraction_theta_max 0.222
_diffrn_measurement_method       ω-scan
_diffrn_radiation_wavelength     0.71442
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.239
_diffrn_reflns_Laue_measured_fraction_max 0.222
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            309
_diffrn_reflns_point_group_measured_fraction_full 0.239
_diffrn_reflns_point_group_measured_fraction_max 0.222
_diffrn_reflns_theta_full        25.382
_diffrn_reflns_theta_max         26.505
_diffrn_reflns_theta_min         3.906
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.252
_exptl_absorpt_correction_T_min  0.174
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; Absorb7 and Absorb-GUI, Angel and Gonzalez-Platas (2013)
  J. Appl. Cryst. 46:252-254
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_description       prism
_exptl_crystal_F_000             192
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.091
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.1358
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4099
_refine_ls_wR_factor_ref         0.4384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                114
_reflns_number_total             147
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4ce02550d1.cif
_cod_data_source_block           6.2GPa_P21c
_cod_depositor_comments
'Adding full bibliography for 7219427--7219430.cif.'
_cod_database_code               7219429
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelxl_version_number           2014/6
_shelx_res_file
;
TITL
CELL  0.71442  5.25928 13.10096  4.74083 90.00000 94.32190 90.00000
ZERR 4  0.00144  0.03829  0.00103  0.00000  0.02600  0.00000
LATT 1
SYMM -X, Y+ 0.50000, -Z+ 0.50000
SFAC C H N O
UNIT 12 28 4 8
PLAN 30
FMAP 2
L.S. 20
EQIV $1 1+X,Y,Z
EQIV $2 X,1.5-Y,0.5+Z
EQIV $3 1+X,Y,1+Z
HTAB N1 O1_$1
HTAB N1 O2_$2
HTAB N1 O1_$3
SHEL 50 0.8
BOND
BOND $H
CONF
ACTA
WGHT    0.200000
FVAR      18.26500
O1    4   -0.247669    0.660478   -0.144395    11.00000    0.02274
O2    4    0.172260    0.669161   -0.197181    11.00000    0.01708
C1    1   -0.022221    0.647346   -0.061407    11.00000    0.02396
C2    1    0.027765    0.587145    0.218820    11.00000    0.02504
AFIX  23
H2A   2   -0.051641    0.623443    0.367379    11.00000   -1.20000
H2B   2   -0.054463    0.521038    0.197224    11.00000   -1.20000
AFIX   0
C3    1    0.284174    0.572068    0.304436    11.00000    0.03011
AFIX  23
H3B   2    0.350162    0.522078    0.177852    11.00000   -1.20000
H3A   2    0.292180    0.541368    0.491082    11.00000   -1.20000
AFIX   0
N1    3    0.470657    0.664653    0.318746    11.00000    0.01177
AFIX  33
H1C   2    0.626749    0.643443    0.376438    11.00000   -1.50000
H1B   2    0.472899    0.692709    0.147978    11.00000   -1.50000
H1A   2    0.418843    0.710692    0.439997    11.00000   -1.50000
AFIX   0
HKLF 4

REM
REM R1 =  0.1358 for     114 Fo > 4sig(Fo)  and  0.1544 for all     147 data
REM     25 parameters refined using      0 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  0.563,  deepest hole -0.427,  1-sigma level  0.118
Q1    1   0.3710  0.6679  0.3399  11.00000  0.05    0.56
Q2    1   0.0811  0.6780 -0.1618  11.00000  0.05    0.50
Q3    1  -0.3296  0.6595 -0.1344  11.00000  0.05    0.34
Q4    1   0.0045  0.6602  0.2216  11.00000  0.05    0.34
Q5    1   0.0000  0.5000  0.0000  10.50000  0.05    0.30
Q6    1   0.6192  0.6630  0.1645  11.00000  0.05    0.30
Q7    1   0.7646  0.6638  0.5588  11.00000  0.05    0.24
Q8    1   0.1764  0.6574  0.2660  11.00000  0.05    0.23
Q9    1   0.1297  0.5718  0.2254  11.00000  0.05    0.21
Q10   1  -0.1151  0.5316  0.2896  11.00000  0.05    0.21
Q11   1   0.4954  0.5624  0.3811  11.00000  0.05    0.20
Q12   1   0.5847  0.6835  0.4903  11.00000  0.05    0.19
Q13   1   0.1656  0.6213  0.5447  11.00000  0.05    0.18
Q14   1  -0.4983  0.6815 -0.1330  11.00000  0.05    0.17
Q15   1   0.3356  0.6606 -0.3636  11.00000  0.05    0.16
Q16   1   0.4351  0.6266  0.1157  11.00000  0.05    0.15
Q17   1   0.7843  0.7007  0.3093  11.00000  0.05    0.14
Q18   1  -0.1156  0.6778 -0.2438  11.00000  0.05    0.14
Q19   1  -0.1202  0.6392 -0.0527  11.00000  0.05    0.12
Q20   1   0.0024  0.6700  0.5327  11.00000  0.05    0.10
;
_shelx_res_checksum              73277
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
O1 O -0.2477(18) 0.6605(16) -0.144(2) 0.023(4) Uiso 1 1 d . .
O2 O 0.1723(12) 0.6692(17) -0.1972(17) 0.017(4) Uiso 1 1 d . .
C1 C -0.022(3) 0.647(2) -0.061(3) 0.024(5) Uiso 1 1 d . .
C2 C 0.028(2) 0.587(3) 0.219(2) 0.025(4) Uiso 1 1 d . .
H2A H -0.0516 0.6234 0.3674 0.030 Uiso 1 1 calc R U
H2B H -0.0545 0.5210 0.1972 0.030 Uiso 1 1 calc R U
C3 C 0.284(2) 0.572(3) 0.304(3) 0.030(5) Uiso 1 1 d . .
H3B H 0.3502 0.5221 0.1779 0.036 Uiso 1 1 calc R U
H3A H 0.2922 0.5414 0.4911 0.036 Uiso 1 1 calc R U
N1 N 0.4707(14) 0.665(2) 0.3187(18) 0.012(4) Uiso 1 1 d . .
H1C H 0.6267 0.6434 0.3764 0.018 Uiso 1 1 calc R U
H1B H 0.4729 0.6927 0.1480 0.018 Uiso 1 1 calc R U
H1A H 0.4188 0.7107 0.4400 0.018 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
O1 C1 O2 126.4(17)
O1 C1 C2 116.2(17)
O2 C1 C2 117.0(14)
C3 C2 C1 114.8(19)
C3 C2 H2A 108.6
C1 C2 H2A 108.6
C3 C2 H2B 108.6
C1 C2 H2B 108.6
H2A C2 H2B 107.5
C2 C3 N1 120(3)
C2 C3 H3B 107.4
N1 C3 H3B 107.4
C2 C3 H3A 107.4
N1 C3 H3A 107.4
H3B C3 H3A 106.9
C3 N1 H1C 109.5
C3 N1 H1B 109.5
H1C N1 H1B 109.5
C3 N1 H1A 109.5
H1C N1 H1A 109.5
H1B N1 H1A 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C1 1.233(18)
O2 C1 1.28(2)
C1 C2 1.55(3)
C2 C3 1.39(2)
C2 H2A 0.9700
C2 H2B 0.9700
C3 N1 1.56(4)
C3 H3B 0.9700
C3 H3A 0.9700
N1 H1C 0.8900
N1 H1B 0.8900
N1 H1A 0.8900
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1B O1 0.89 2.14 2.740(15) 124.4 1_655
N1 H1A O2 0.89 2.11 2.68(3) 121.2 4_576
N1 H1C O1 0.89 2.33 2.847(11) 117.2 1_656
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 C3 179(3)
O2 C1 C2 C3 6(5)
C1 C2 C3 N1 51(3)
