#------------------------------------------------------------------------------
#$Date: 2014-10-25 20:23:10 +0300 (Sat, 25 Oct 2014) $
#$Revision: 125873 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/51/2105153.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_2105153
loop_
_publ_author_name
'Tumanov, Nikolay A.'
'Boldyreva, Elena V.'
_publ_section_title
;
X-ray diffraction and Raman study of DL-alanine at high
pressure: revision of phase transitions
;
_journal_coeditor_code GP5051
_journal_issue 4
_journal_name_full 'Acta Crystallographica Section B'
_journal_page_first 412
_journal_page_last 423
_journal_volume 68
_journal_year 2012
_chemical_formula_moiety 'C3 H7 N O2'
_chemical_formula_sum 'C3 H7 N O2'
_chemical_formula_weight 89.10
_chemical_name_common DL-alanine
_chemical_name_systematic 'DL-2-Aminopropionic Acid '
_space_group_IT_number 33
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2c -2n'
_symmetry_space_group_name_H-M 'P n a 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.537(3)
_cell_length_b 5.554(3)
_cell_length_c 5.6456(8)
_cell_measurement_reflns_used 1408
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 30.9919
_cell_measurement_theta_min 3.6016
_cell_volume 361.8(2)
_computing_cell_refinement 'CrysAlis Pro (Oxford Diffraction Ltd, 2010)'
_computing_data_collection 'CrysAlis Pro (Oxford Diffraction Ltd, 2010)'
_computing_data_reduction 'CrysAlis Pro (Oxford Diffraction Ltd, 2010)'
_computing_molecular_graphics 'Mercury (Macrae et al., 2008)'
_computing_publication_material
;
Mercury (Macrae et al., 2008),
PLATON (Spek, 2009),
enCIFer (Allen et al., 2004)
;
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.437
_diffrn_measured_fraction_theta_max 0.437
_diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra R'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0745
_diffrn_reflns_av_sigmaI/netI 0.0537
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_k_min -4
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 3018
_diffrn_reflns_theta_full 31.06
_diffrn_reflns_theta_max 31.06
_diffrn_reflns_theta_min 5.05
_exptl_absorpt_coefficient_mu 0.137
_exptl_absorpt_correction_T_max 0.478
_exptl_absorpt_correction_T_min 0.408
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
Absorb6.1 (R. J. Angel, 2004)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.636
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 192
_exptl_crystal_size_max 0.16
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.157
_refine_diff_density_min -0.151
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.048
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 57
_refine_ls_number_reflns 499
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.047
_refine_ls_R_factor_all 0.0599
_refine_ls_R_factor_gt 0.0419
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0715
_refine_ls_wR_factor_ref 0.0787
_reflns_number_gt 396
_reflns_number_total 499
_reflns_threshold_expression I>2\s(I)
_iucr_refine_instructions_details
;
TITL DLALA_50KBAR_NV_OU IN PNA2(1)
CELL 0.71073 11.53670 5.55404 5.64560 90.00000 90.00000 90.00000
ZERR 3 0.00267 0.00324 0.00079 0.00000 0.00000 0.00000
LATT -1
SYMM -X, -Y, Z+ 0.50000
SYMM -X+ 0.50000, Y+ 0.50000, Z+ 0.50000
SYMM X+ 0.50000, -Y+ 0.50000, Z
SFAC C H N O
UNIT 12 28 4 8
L.S. 10
PLAN 30
FMAP 2
ACTA
CONF
BOND $H
EQIV $1 x,y,-1+z
EQIV $2 1-x,1-y,-1/2+z
EQIV $3 3/2-x,1/2+y,-1/2+z
HTAB N1 O2_$2
HTAB N1 O1_$1
HTAB N1 O2_$1
HTAB N1 O1_$3
WGHT 0.032700
FVAR 6.63726
O2 4 0.594041 0.483393 0.610241 11.00000 0.03147 0.03110 =
0.02086 -0.00136 0.00027 0.00588
O1 4 0.683840 0.157504 0.747428 11.00000 0.03347 0.02695 =
0.01774 0.00298 -0.00037 0.00781
C1 1 0.645184 0.289003 0.583192 11.00000 0.01133 0.03263 =
0.02143 0.00289 0.00206 -0.00171
C2 1 0.662434 0.190034 0.332543 11.00000 0.02033 0.02901 =
0.01394 0.00085 -0.00108 -0.00011
AFIX 13
H2 2 0.744181 0.146780 0.312131 11.00000 -1.20000
AFIX 0
C3 1 0.589546 -0.028611 0.288180 11.00000 0.03502 0.03819 =
0.02225 0.00168 -0.00305 -0.00288
AFIX 137
H3B 2 0.608030 -0.094265 0.135482 11.00000 -1.20000
H3A 2 0.509074 0.015170 0.292405 11.00000 -1.20000
H3C 2 0.604830 -0.146841 0.408225 11.00000 -1.20000
AFIX 0
N1 3 0.632344 0.377828 0.158614 11.00000 0.02458 0.03640 =
0.01442 -0.00164 0.00047 -0.00414
AFIX 137
H1C 2 0.677207 0.506118 0.181385 11.00000 -1.20000
H1A 2 0.558367 0.419420 0.176642 11.00000 -1.20000
H1B 2 0.643289 0.321337 0.012795 11.00000 -1.20000
HKLF 4
REM DLALA_50KBAR_NV_OU IN PNA2(1)
REM R1 = 0.0419 for 396 Fo > 4sig(Fo) and 0.0599 for all 499 data
REM 57 parameters refined using 1 restraints
END
WGHT 0.0327 0.0000
REM Highest difference peak 0.157, deepest hole -0.151, 1-sigma level 0.042
Q1 1 0.7327 0.6226 0.2416 11.00000 0.05 0.16
Q2 1 0.5797 0.5565 0.1223 11.00000 0.05 0.15
Q3 1 0.5431 -0.0949 0.1092 11.00000 0.05 0.14
Q4 1 0.7638 0.4885 0.2474 11.00000 0.05 0.14
Q5 1 0.3863 0.1814 0.3094 11.00000 0.05 0.14
Q6 1 0.5935 0.4833 0.5336 11.00000 0.05 0.13
Q7 1 0.6475 0.0732 0.1165 11.00000 0.05 0.13
Q8 1 0.5536 0.5966 0.7277 11.00000 0.05 0.13
Q9 1 0.7651 0.4510 0.1488 11.00000 0.05 0.12
Q10 1 0.5213 0.5423 0.6130 11.00000 0.05 0.12
Q11 1 0.6200 -0.1906 0.6452 11.00000 0.05 0.12
Q12 1 0.7178 0.3793 0.3121 11.00000 0.05 0.11
Q13 1 0.7205 0.3480 0.1849 11.00000 0.05 0.11
Q14 1 0.6445 0.3188 0.7532 11.00000 0.05 0.11
Q15 1 0.5461 0.6432 0.6069 11.00000 0.05 0.11
Q16 1 0.7349 0.0273 0.4954 11.00000 0.05 0.11
Q17 1 0.7161 0.3172 0.6293 11.00000 0.05 0.11
Q18 1 0.6190 0.5277 0.8130 11.00000 0.05 0.10
Q19 1 0.5804 0.5095 0.4460 11.00000 0.05 0.10
Q20 1 0.6000 0.1026 0.7247 11.00000 0.05 0.10
Q21 1 0.6948 -0.2253 0.1007 11.00000 0.05 0.10
Q22 1 0.6355 0.5692 0.7932 11.00000 0.05 0.10
Q23 1 0.6587 0.2646 0.4590 11.00000 0.05 0.10
Q24 1 0.5970 0.4878 0.6821 11.00000 0.05 0.10
Q25 1 0.5574 0.6519 0.8333 11.00000 0.05 0.09
Q26 1 0.5592 -0.0037 0.4214 11.00000 0.05 0.09
Q27 1 0.6815 0.1577 0.6658 11.00000 0.05 0.09
Q28 1 0.4981 0.4828 0.5173 11.00000 0.05 0.09
Q29 1 0.5404 0.3493 0.0215 11.00000 0.05 0.09
Q30 1 0.5922 0.1555 0.2880 11.00000 0.05 0.09
;
_[local]_cod_data_source_file gp5051.cif
_[local]_cod_data_source_block dlala_50kbar
_cod_original_cell_volume 361.7(2)
_cod_database_code 2105153
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
O O2 0.5940(2) 0.4834(7) 0.6102(3) 0.0278(9) Uani d . 1 1
O O1 0.68384(16) 0.1575(5) 0.7474(3) 0.0261(8) Uani d . 1 1
C C1 0.6452(2) 0.2890(9) 0.5832(5) 0.0218(14) Uani d . 1 1
C C2 0.6624(2) 0.1900(9) 0.3325(4) 0.0211(14) Uani d . 1 1
H H2 0.7442 0.1468 0.3121 0.025 Uiso calc R 1 1
C C3 0.5895(3) -0.0286(11) 0.2882(6) 0.0318(17) Uani d . 1 1
H H3B 0.6080 -0.0943 0.1355 0.038 Uiso calc R 1 1
H H3A 0.5091 0.0152 0.2924 0.038 Uiso calc R 1 1
H H3C 0.6048 -0.1468 0.4082 0.038 Uiso calc R 1 1
N N1 0.6323(2) 0.3778(7) 0.1586(3) 0.0251(11) Uani d . 1 1
H H1C 0.6772 0.5061 0.1814 0.030 Uiso calc R 1 1
H H1A 0.5584 0.4194 0.1766 0.030 Uiso calc R 1 1
H H1B 0.6433 0.3213 0.0128 0.030 Uiso calc R 1 1
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
O2 0.0315(13) 0.031(3) 0.0209(11) 0.0059(11) 0.0003(9) -0.0014(13)
O1 0.0335(14) 0.027(3) 0.0177(9) 0.0078(9) -0.0004(8) 0.0030(14)
C1 0.0113(19) 0.033(5) 0.0214(16) -0.0017(12) 0.0021(12) 0.0029(19)
C2 0.0203(19) 0.029(5) 0.0139(14) -0.0001(14) -0.0011(9) 0.0009(18)
C3 0.035(2) 0.038(6) 0.0222(17) -0.0029(15) -0.0030(12) 0.002(2)
N1 0.0246(16) 0.036(4) 0.0144(12) -0.0041(11) 0.0005(9) -0.0016(16)
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 125.6(3)
O2 C1 C2 119.2(3)
O1 C1 C2 115.2(3)
N1 C2 C3 109.3(3)
N1 C2 C1 109.3(3)
C3 C2 C1 111.9(3)
N1 C2 H2 108.8
C3 C2 H2 108.8
C1 C2 H2 108.8
C2 C3 H3B 109.5
C2 C3 H3A 109.5
H3B C3 H3A 109.5
C2 C3 H3C 109.5
H3B C3 H3C 109.5
H3A C3 H3C 109.5
C2 N1 H1C 109.5
C2 N1 H1A 109.5
H1C N1 H1A 109.5
C2 N1 H1B 109.5
H1C N1 H1B 109.5
H1A N1 H1B 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O2 C1 1.240(6)
O1 C1 1.262(4)
C1 C2 1.531(4)
C2 N1 1.474(5)
C2 C3 1.498(7)
C2 H2 0.9800
C3 H3B 0.9600
C3 H3A 0.9600
C3 H3C 0.9600
N1 H1C 0.8900
N1 H1A 0.8900
N1 H1B 0.8900
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A O2 2_664 0.89 1.88 2.737(3) 161.8
N1 H1B O1 1_554 0.89 1.81 2.691(3) 167.8
N1 H1B O2 1_554 0.89 2.51 3.182(3) 132.8
N1 H1C O1 3_654 0.89 1.85 2.676(4) 153.9
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 N1 11.1(5)
O1 C1 C2 N1 -170.2(3)
O2 C1 C2 C3 -110.0(5)
O1 C1 C2 C3 68.6(4)
_journal_paper_doi 10.1107/S0108768112028972