#------------------------------------------------------------------------------ #$Date: 2012-09-06 16:54:02 +0300 (Thu, 06 Sep 2012) $ #$Revision: 65853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/51/2105143.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_2105143 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 11.994(2) _cell_length_b 6.0103(16) _cell_length_c 5.8421(5) _cell_measurement_reflns_used 1621 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 31.0477 _cell_measurement_theta_min 3.4803 _cell_volume 421.14(14) _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 0.478 _diffrn_measured_fraction_theta_max 0.478 _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 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 3719 _diffrn_reflns_theta_full 31.12 _diffrn_reflns_theta_max 31.12 _diffrn_reflns_theta_min 3.79 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_T_max 0.478 _exptl_absorpt_correction_T_min 0.399 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; Absorb6.1 (R. J. Angel, 2004) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.405 _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 0.108 _refine_diff_density_min -0.111 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 57 _refine_ls_number_reflns 647 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0395 _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^)+(0.0342P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.0771 _reflns_number_gt 487 _reflns_number_total 647 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL DLALA_01KBAR_NV_OU IN PNA2(1) CELL 0.71073 11.99356 6.01026 5.84213 90.00000 90.00000 90.00000 ZERR 4 0.00237 0.00164 0.00052 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 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 0.034200 FVAR 6.34054 O2 4 0.588526 0.483841 0.604227 11.00000 0.03936 0.05045 = 0.02748 -0.00495 0.00462 0.01714 O1 4 0.686380 0.198617 0.740601 11.00000 0.04352 0.04848 = 0.01810 0.00251 -0.00175 0.00615 C1 1 0.645461 0.313135 0.581523 11.00000 0.02113 0.05025 = 0.01752 -0.00280 0.00250 -0.00189 C2 1 0.663138 0.218337 0.338587 11.00000 0.02804 0.03133 = 0.01727 -0.00042 -0.00159 0.00262 AFIX 13 H2 2 0.741528 0.174761 0.323398 11.00000 -1.20000 AFIX 0 C3 1 0.592580 0.018987 0.292965 11.00000 0.04899 0.04695 = 0.02516 -0.00159 0.00076 -0.00539 AFIX 137 H3B 2 0.606106 -0.033295 0.140197 11.00000 -1.20000 H3C 2 0.515365 0.058120 0.308896 11.00000 -1.20000 H3A 2 0.610835 -0.096228 0.400427 11.00000 -1.20000 AFIX 0 N1 3 0.639123 0.394812 0.165567 11.00000 0.03024 0.03842 = 0.01879 0.00107 -0.00101 0.00014 AFIX 137 H1C 2 0.684591 0.509778 0.188063 11.00000 -1.20000 H1B 2 0.568717 0.439458 0.179936 11.00000 -1.20000 H1A 2 0.649747 0.340382 0.025579 11.00000 -1.20000 HKLF 4 REM DLALA_01KBAR_NV_OU IN PNA2(1) REM R1 = 0.0395 for 487 Fo > 4sig(Fo) and 0.0637 for all 647 data REM 57 parameters refined using 1 restraints END WGHT 0.0342 0.0000 REM Highest difference peak 0.108, deepest hole -0.111, 1-sigma level 0.030 Q1 1 0.6564 0.2327 0.4635 11.00000 0.05 0.11 Q2 1 0.7648 0.5199 0.2662 11.00000 0.05 0.10 Q3 1 0.6480 0.2912 0.4413 11.00000 0.05 0.10 Q4 1 0.6220 -0.1947 0.2361 11.00000 0.05 0.10 Q5 1 0.5457 0.6329 0.6126 11.00000 0.05 0.10 Q6 1 0.5380 0.4131 0.6108 11.00000 0.05 0.10 Q7 1 0.6233 0.6874 0.6628 11.00000 0.05 0.10 Q8 1 0.6908 0.4477 0.7558 11.00000 0.05 0.09 Q9 1 0.6568 0.6966 0.1885 11.00000 0.05 0.09 Q10 1 0.6826 -0.0243 0.7246 11.00000 0.05 0.09 Q11 1 0.6958 0.3112 0.3158 11.00000 0.05 0.09 Q12 1 0.6416 0.2090 0.0182 11.00000 0.05 0.09 Q13 1 0.6986 0.3159 0.1719 11.00000 0.05 0.09 Q14 1 0.6621 -0.0871 0.1832 11.00000 0.05 0.09 Q15 1 0.4794 0.2838 0.5984 11.00000 0.05 0.08 Q16 1 0.6162 0.1142 0.4545 11.00000 0.05 0.08 Q17 1 0.5980 0.1468 0.7496 11.00000 0.05 0.08 Q18 1 0.7401 0.4416 0.1167 11.00000 0.05 0.08 Q19 1 0.5237 -0.1918 0.2425 11.00000 0.05 0.08 Q20 1 0.4414 0.1841 0.1962 11.00000 0.05 0.08 Q21 1 0.5405 0.4910 0.7563 11.00000 0.05 0.08 Q22 1 0.5852 0.6173 0.1178 11.00000 0.05 0.08 Q23 1 0.7445 0.2762 0.7297 11.00000 0.05 0.08 Q24 1 0.6030 0.0274 0.1829 11.00000 0.05 0.08 Q25 1 0.4167 0.0071 0.3912 11.00000 0.05 0.08 Q26 1 0.5955 0.4433 0.7358 11.00000 0.05 0.08 Q27 1 0.5780 0.5690 0.6846 11.00000 0.05 0.08 Q28 1 0.5778 -0.0980 0.0830 11.00000 0.05 0.07 Q29 1 0.5385 -0.2196 0.0872 11.00000 0.05 0.07 Q30 1 0.7684 0.3469 0.3725 11.00000 0.05 0.07 ; _[local]_cod_data_source_file gp5051.cif _[local]_cod_data_source_block dlala_01kbar _cod_original_cell_volume 421.13(15) _cod_database_code 2105143 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 0.58853(18) 0.4838(4) 0.6042(3) 0.0391(6) Uani d . 1 1 O O1 0.68638(15) 0.1986(3) 0.7406(2) 0.0367(5) Uani d . 1 1 C C1 0.6455(2) 0.3131(6) 0.5815(4) 0.0296(7) Uani d . 1 1 C C2 0.6631(2) 0.2183(5) 0.3386(3) 0.0255(7) Uani d . 1 1 H H2 0.7415 0.1748 0.3234 0.031 Uiso calc R 1 1 C C3 0.5926(3) 0.0190(6) 0.2930(4) 0.0404(9) Uani d . 1 1 H H3B 0.6061 -0.0333 0.1402 0.048 Uiso calc R 1 1 H H3C 0.5154 0.0581 0.3089 0.048 Uiso calc R 1 1 H H3A 0.6108 -0.0962 0.4004 0.048 Uiso calc R 1 1 N N1 0.63912(17) 0.3948(4) 0.1656(3) 0.0292(6) Uani d . 1 1 H H1C 0.6846 0.5098 0.1881 0.035 Uiso calc R 1 1 H H1B 0.5687 0.4395 0.1799 0.035 Uiso calc R 1 1 H H1A 0.6497 0.3404 0.0256 0.035 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 0.0394(16) 0.0505(19) 0.0275(10) 0.0171(9) 0.0046(10) -0.0049(8) O1 0.0435(15) 0.048(2) 0.0181(6) 0.0061(9) -0.0017(9) 0.0025(10) C1 0.021(2) 0.050(3) 0.0175(10) -0.0019(11) 0.0025(10) -0.0028(13) C2 0.028(2) 0.031(3) 0.0173(10) 0.0026(10) -0.0016(10) -0.0004(12) C3 0.049(3) 0.047(3) 0.0252(15) -0.0054(13) 0.0008(12) -0.0016(14) N1 0.0302(15) 0.038(2) 0.0188(8) 0.0001(9) -0.0010(8) 0.0011(9) 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 126.1(2) O2 C1 C2 118.6(2) O1 C1 C2 115.1(2) C3 C2 N1 109.9(2) C3 C2 C1 112.5(2) N1 C2 C1 109.5(2) C3 C2 H2 108.3 N1 C2 H2 108.3 C1 C2 H2 108.3 C2 C3 H3B 109.5 C2 C3 H3C 109.5 H3B C3 H3C 109.5 C2 C3 H3A 109.5 H3B C3 H3A 109.5 H3C C3 H3A 109.5 C2 N1 H1C 109.5 C2 N1 H1B 109.5 H1C N1 H1B 109.5 C2 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 O2 C1 1.240(4) O1 C1 1.256(3) C1 C2 1.544(3) C2 C3 1.491(4) C2 N1 1.493(3) C2 H2 0.9800 C3 H3B 0.9600 C3 H3C 0.9600 C3 H3A 0.9600 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_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1B O2 2_664 0.89 1.99 2.849(3) 161.3 N1 H1A O1 1_554 0.89 1.92 2.806(2) 172.8 N1 H1A O2 1_554 0.89 2.71 3.378(3) 132.8 N1 H1C O1 3_654 0.89 1.94 2.812(2) 164.7 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 O2 C1 C2 C3 -103.4(4) O1 C1 C2 C3 72.7(4) O2 C1 C2 N1 19.1(4) O1 C1 C2 N1 -164.8(2)