#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:59:10 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180525 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/94/7219428.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_7219428
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      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.4310(8)
_cell_length_b                   12.826(16)
_cell_length_c                   5.6952(5)
_cell_measurement_reflns_used    229
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6250
_cell_measurement_theta_min      4.3470
_cell_volume                     688.9(9)
_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)'
_diffrn_ambient_pressure         6300000(50000)
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.310
_diffrn_measured_fraction_theta_max 0.266
_diffrn_measurement_method       ω-scan
_diffrn_radiation_wavelength     0.71442
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.310
_diffrn_reflns_Laue_measured_fraction_max 0.266
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            567
_diffrn_reflns_point_group_measured_fraction_full 0.310
_diffrn_reflns_point_group_measured_fraction_max 0.266
_diffrn_reflns_theta_full        25.382
_diffrn_reflns_theta_max         27.896
_diffrn_reflns_theta_min         4.496
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.253
_exptl_absorpt_correction_T_min  0.169
_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    1.718
_exptl_crystal_description       prism
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         217
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0550
_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)+(0.1164P)²+0.0453P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                195
_reflns_number_total             217
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4ce02550d1.cif
_cod_data_source_block           6.3GPa_Pbca
_cod_depositor_comments
'Adding full bibliography for 7219427--7219430.cif.'
_cod_database_code               7219428
#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  9.43103 12.82636  5.69520 90.00000 90.00000 90.00000
ZERR 8  0.00077  0.01593  0.00051  0.00000  0.00000  0.00000
LATT 1
SYMM -X+ 0.50000, -Y, Z+ 0.50000
SYMM X+ 0.50000, -Y+ 0.50000, -Z
SYMM -X, Y+ 0.50000, -Z+ 0.50000
SFAC C H N O
UNIT 48 112 16 32
PLAN 30
FMAP 2
L.S. 20
EQIV $1 0.5+X,Y,-0.5-Z
EQIV $2 -X,-Y,-Z
EQIV $3 0.5+X,Y,0.5-Z
HTAB N1 O1_$1
HTAB N1 O1_$2
HTAB N1 O2_$3
BOND
BOND $H
SIMU
DELU
CONF
ACTA
WGHT    0.116400    0.045300
FVAR      13.24903
O1    4   -0.136871    0.106713   -0.004359    11.00000    0.02518    0.03245 =
         0.02612   -0.00614    0.00024   -0.00392
O2    4    0.031841    0.083227    0.258613    11.00000    0.03032    0.02437 =
         0.02438    0.00974    0.00291    0.00551
C1    1   -0.010959    0.113926    0.065557    11.00000    0.02290    0.03548 =
         0.02102   -0.00480    0.00228    0.00502
C2    1    0.092336    0.171224   -0.095647    11.00000    0.02720    0.02559 =
         0.01783    0.00300   -0.00039    0.00176
AFIX  23
H2A   2    0.089203    0.140131   -0.250817    11.00000   -1.20000
H2B   2    0.063345    0.243507   -0.109884    11.00000   -1.20000
AFIX   0
C3    1    0.243004    0.166603   -0.002647    11.00000    0.02490    0.00804 =
         0.02652    0.00103   -0.00197   -0.00428
AFIX  23
H3A   2    0.299505    0.219838   -0.079327    11.00000   -1.20000
H3B   2    0.242452    0.181295    0.164425    11.00000   -1.20000
AFIX   0
N1    3    0.307713    0.064759   -0.042795    11.00000    0.02229    0.01205 =
         0.01953   -0.00239    0.00245    0.00638
AFIX 137
H1A   2    0.338518    0.060954   -0.190257    11.00000   -1.50000
H1B   2    0.243729    0.014984   -0.017732    11.00000   -1.50000
H1C   2    0.380341    0.056249    0.055127    11.00000   -1.50000
REM
REM R1    0.0550 FOR     195 FO > 4SIG(FO)  AND  0.0594 FOR ALL     217 DATA
REM     56 PARAMETERS REFINED USING     40 RESTRAINTS
REM HIGHEST DIFFERENCE PEAK  0.163,  DEEPEST HOLE -0.201,  1-SIGMA LEVEL  0.059
AFIX   0
HKLF 4

REM
REM R1 =  0.0550 for     195 Fo > 4sig(Fo)  and  0.0594 for all     217 data
REM     56 parameters refined using     40 restraints

END

WGHT      0.1164      0.0453

REM Highest difference peak  0.163,  deepest hole -0.201,  1-sigma level  0.059
Q1    1   0.3021  0.1286 -0.2033  11.00000  0.05    0.16
Q2    1   0.0401  0.0612  0.4626  11.00000  0.05    0.15
Q3    1   0.2983  0.2602  0.0056  11.00000  0.05    0.14
Q4    1   0.0247  0.1071  0.4422  11.00000  0.05    0.14
Q5    1   0.0412  0.1126  0.2277  11.00000  0.05    0.13
Q6    1   0.3639  0.0587 -0.2980  11.00000  0.05    0.12
Q7    1   0.0989  0.1114  0.4906  11.00000  0.05    0.12
Q8    1   0.1352  0.1653 -0.2746  11.00000  0.05    0.12
Q9    1   0.1843  0.0266 -0.0044  11.00000  0.05    0.10
Q10   1   0.4232  0.2668 -0.0398  11.00000  0.05    0.09
Q11   1  -0.0635  0.2881 -0.2495  11.00000  0.05    0.09
Q12   1   0.1930  0.3273 -0.0084  11.00000  0.05    0.09
Q13   1   0.1827  0.2892 -0.0235  11.00000  0.05    0.09
Q14   1   0.0404  0.1498  0.0085  11.00000  0.05    0.08
Q15   1   0.1659 -0.0050 -0.2139  11.00000  0.05    0.08
Q16   1  -0.2875  0.0979  0.0014  11.00000  0.05    0.07
Q17   1   0.3101  0.0304 -0.0014  11.00000  0.05    0.07
Q18   1   0.0881  0.0643 -0.0269  11.00000  0.05    0.06
Q19   1   0.3601  0.1774 -0.0028  11.00000  0.05    0.06
Q20   1   0.2631  0.0761  0.1741  11.00000  0.05    0.05
Q21   1   0.1435  0.1908 -0.0234  11.00000  0.05    0.03
;
_shelx_res_checksum              3950
#END Tags that were not found in dictionaries
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'
'-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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
O1 O -0.1369(2) 0.1067(5) -0.0044(4) 0.028(5) Uani 1 1 d . U
O2 O 0.0318(2) 0.0832(5) 0.2586(4) 0.026(6) Uani 1 1 d . U
C1 C -0.0110(3) 0.1139(8) 0.0656(6) 0.026(6) Uani 1 1 d . U
C2 C 0.0923(3) 0.1712(8) -0.0956(5) 0.024(6) Uani 1 1 d . U
H2A H 0.0892 0.1401 -0.2508 0.028 Uiso 1 1 calc R U
H2B H 0.0633 0.2435 -0.1099 0.028 Uiso 1 1 calc R U
C3 C 0.2430(3) 0.1666(8) -0.0026(6) 0.020(5) Uani 1 1 d . U
H3A H 0.2995 0.2198 -0.0793 0.024 Uiso 1 1 calc R U
H3B H 0.2425 0.1813 0.1644 0.024 Uiso 1 1 calc R U
N1 N 0.3077(3) 0.0648(6) -0.0428(4) 0.018(5) Uani 1 1 d . U
H1A H 0.3385 0.0610 -0.1903 0.027 Uiso 1 1 calc R U
H1B H 0.2437 0.0150 -0.0177 0.027 Uiso 1 1 calc R U
H1C H 0.3803 0.0562 0.0551 0.027 Uiso 1 1 calc R 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
O1 0.0252(13) 0.032(16) 0.0261(16) -0.0061(18) 0.0002(7) -0.004(2)
O2 0.0303(13) 0.024(17) 0.0244(15) 0.010(2) 0.0029(7) 0.006(2)
C1 0.0229(15) 0.035(19) 0.0210(18) -0.005(3) 0.0023(9) 0.005(3)
C2 0.0272(15) 0.026(18) 0.0178(17) 0.003(3) -0.0004(9) 0.002(2)
C3 0.0249(15) 0.008(14) 0.0265(19) 0.001(3) -0.0020(11) -0.004(3)
N1 0.0223(14) 0.012(15) 0.0195(15) -0.002(3) 0.0024(9) 0.006(3)
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
O2 C1 O1 124.6(5)
O2 C1 C2 118.7(3)
O1 C1 C2 116.6(4)
C3 C2 C1 111.6(4)
C3 C2 H2A 109.3
C1 C2 H2A 109.3
C3 C2 H2B 109.3
C1 C2 H2B 109.3
H2A C2 H2B 108.0
N1 C3 C2 111.8(7)
N1 C3 H3A 109.3
C2 C3 H3A 109.3
N1 C3 H3B 109.3
C2 C3 H3B 109.3
H3A C3 H3B 107.9
C3 N1 H1A 109.5
C3 N1 H1B 109.5
H1A N1 H1B 109.5
C3 N1 H1C 109.5
H1A N1 H1C 109.5
H1B N1 H1C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C1 1.256(4)
O2 C1 1.236(5)
C1 C2 1.527(8)
C2 C3 1.518(4)
C2 H2A 0.9700
C2 H2B 0.9700
C3 N1 1.460(12)
C3 H3A 0.9700
C3 H3B 0.9700
N1 H1A 0.8900
N1 H1B 0.8900
N1 H1C 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 H1A O1 0.89 1.85 2.686(4) 155.6 6_655
N1 H1B O1 0.89 1.86 2.740(8) 168.2 5
N1 H1C O2 0.89 1.81 2.673(3) 161.8 6_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
O2 C1 C2 C3 8.9(11)
O1 C1 C2 C3 -175.0(8)
C1 C2 C3 N1 76.1(6)
