#------------------------------------------------------------------------------ #$Date: 2017-10-13 06:28:26 +0100 (Fri, 13 Oct 2017) $ #$Revision: 201972 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/51/2105107.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_2105107 loop_ _publ_author_name 'Zakharov, Boris A.' 'Kolesov, Boris A.' 'Boldyreva, Elena V.' _publ_section_title ; Effect of pressure on crystalline L- and DL-serine: revisited by a combined single-crystal X-ray diffraction at a laboratory source and polarized Raman spectroscopy study ; _journal_coeditor_code GP5049 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 275 _journal_page_last 286 _journal_paper_doi 10.1107/S0108768112015960 _journal_volume 68 _journal_year 2012 _chemical_formula_moiety 'C3 H7 N O3' _chemical_formula_sum 'C3 H7 N O3' _chemical_formula_weight 105.10 _chemical_name_common L-serine _chemical_name_systematic ; (S)-2-amino-3-hydroxypropanoic acid ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 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 5.5741(17) _cell_length_b 8.436(9) _cell_length_c 9.088(5) _cell_measurement_reflns_used 713 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 31.6490 _cell_measurement_theta_min 2.2364 _cell_volume 427.3(5) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_molecular_graphics 'Mercury (Macrae et al., 2006)' _computing_publication_material ; Mercury (Macrae et al., 2006), PLATON (Spek, 2009), enCIFer (Allen et al., 2004) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10.3457 _diffrn_measured_fraction_theta_full 0.475 _diffrn_measured_fraction_theta_max 0.475 _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_measurement_method 'rotation method' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_sigmaI/netI 0.1056 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2495 _diffrn_reflns_theta_full 31.72 _diffrn_reflns_theta_max 31.72 _diffrn_reflns_theta_min 3.30 _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_T_max 0.474 _exptl_absorpt_correction_T_min 0.388 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ' Absorb Angel (2004) J. Appl. Cryst. 37:486-492' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 224 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.188 _refine_diff_density_min -0.218 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 66 _refine_ls_number_reflns 638 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.011 _refine_ls_R_factor_all 0.1421 _refine_ls_R_factor_gt 0.0649 _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^)+(0.0615P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1251 _refine_ls_wR_factor_ref 0.1541 _reflns_number_gt 327 _reflns_number_total 638 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL CELL 0.71073 5.57407 8.43552 9.08818 90.00000 90.00000 90.00000 ZERR 4 0.00170 0.00910 0.00480 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 12 28 4 12 PLAN 30 FMAP 2 L.S. 20 EQIV $1 -1+X,Y,Z EQIV $2 -1/2+X,1/2-Y,2-Z EQIV $3 1-X,1/2+Y,1.5-Z EQIV $4 -1/2+X,1/2-Y,1-Z EQIV $11 1-X,-1/2+Y,3/2-Z EQIV $12 -1/2+X,1/2-Y,1-Z HTAB N1 O1_$1 HTAB N1 O2_$1 HTAB N1 O2_$2 HTAB N1 O1_$3 HTAB O3 O3_$4 BOND $H BOND CONF ACTA WGHT 0.061500 FVAR 0.55825 N1 3 0.218573 0.199792 0.816562 11.00000 0.03124 0.03590 = 0.04644 0.00280 0.00169 -0.00005 AFIX 137 H1 2 0.234400 0.290424 0.767378 11.00000 -1.20000 H2 2 0.253507 0.215659 0.910977 11.00000 -1.20000 H3 2 0.068227 0.165314 0.808622 11.00000 -1.20000 AFIX 0 O1 4 0.799681 0.022234 0.756601 11.00000 0.03479 0.05768 = 0.08345 -0.02667 0.00784 0.00363 O2 4 0.677275 0.224588 0.885263 11.00000 0.04355 0.04318 = 0.06030 -0.01782 -0.01198 0.00202 C1 1 0.384597 0.079717 0.754392 11.00000 0.03736 0.04684 = 0.03362 -0.00052 0.00951 -0.01027 AFIX 13 H4 2 0.335493 -0.024243 0.791937 11.00000 -1.20000 AFIX 0 O3 4 0.425211 0.228773 0.530381 11.00000 0.05596 0.06360 = 0.04512 0.00943 0.00178 0.00569 AFIX 147 H5 2 0.305376 0.269277 0.493973 11.00000 -1.20000 AFIX 0 C2 1 0.364689 0.075231 0.589136 11.00000 0.03722 0.04017 = 0.03838 -0.00677 -0.00863 0.00275 AFIX 23 H6 2 0.472828 -0.004259 0.549779 11.00000 -1.20000 H7 2 0.202350 0.047202 0.560833 11.00000 -1.20000 AFIX 0 C3 1 0.642069 0.109031 0.804393 11.00000 0.03622 0.06768 = 0.02522 -0.00089 -0.00137 -0.00580 HKLF 4 REM REM R1 = 0.0649 for 327 Fo > 4sig(Fo) and 0.1421 for all 638 data REM 66 parameters refined using 0 restraints END WGHT 0.0615 0.0000 REM Highest difference peak 0.188, deepest hole -0.218, 1-sigma level 0.050 Q1 1 0.5169 0.3786 0.5374 11.00000 0.05 0.19 Q2 1 0.8086 0.1983 0.9541 11.00000 0.05 0.18 Q3 1 0.5108 0.3039 0.4816 11.00000 0.05 0.17 Q4 1 0.1076 0.4064 0.9417 11.00000 0.05 0.16 Q5 1 1.0403 -0.0706 0.6807 11.00000 0.05 0.16 Q6 1 0.6709 -0.0600 0.7090 11.00000 0.05 0.14 Q7 1 0.5053 0.1042 0.7878 11.00000 0.05 0.14 Q8 1 0.1406 -0.1006 0.5208 11.00000 0.05 0.14 Q9 1 -0.0453 0.1335 0.6796 11.00000 0.05 0.13 Q10 1 0.5265 0.2459 0.5779 11.00000 0.05 0.12 Q11 1 0.5122 -0.0876 0.7555 11.00000 0.05 0.12 Q12 1 0.1137 0.0970 0.5758 11.00000 0.05 0.12 Q13 1 0.8852 0.3117 0.8542 11.00000 0.05 0.12 Q14 1 0.3112 0.2062 0.8925 11.00000 0.05 0.12 Q15 1 0.5690 0.1852 0.5310 11.00000 0.05 0.12 Q16 1 0.5355 0.3171 0.8297 11.00000 0.05 0.12 Q17 1 0.6100 0.2009 0.9595 11.00000 0.05 0.11 Q18 1 0.5762 0.1106 0.4177 11.00000 0.05 0.11 Q19 1 0.9240 -0.0585 0.7516 11.00000 0.05 0.11 Q20 1 0.8713 0.1006 0.8753 11.00000 0.05 0.11 Q21 1 0.4136 -0.0815 0.8378 11.00000 0.05 0.11 Q22 1 0.4480 0.1324 0.4988 11.00000 0.05 0.11 Q23 1 0.7734 0.1687 0.8346 11.00000 0.05 0.11 Q24 1 0.2200 0.0220 0.7189 11.00000 0.05 0.11 Q25 1 0.6125 -0.0895 0.8329 11.00000 0.05 0.11 Q26 1 0.1831 0.2580 0.6189 11.00000 0.05 0.11 Q27 1 0.3575 0.2412 0.8880 11.00000 0.05 0.11 Q28 1 0.5388 0.0489 0.5292 11.00000 0.05 0.10 Q29 1 0.6388 0.2308 0.8412 11.00000 0.05 0.10 Q30 1 0.2895 0.3098 0.6145 11.00000 0.05 0.10 ; _cod_data_source_file gp5049.cif _cod_data_source_block L-serine0.8GPa _cod_database_code 2105107 _cod_database_fobs_code 2105107 loop_ _symmetry_equiv_pos_as_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_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 N N1 0.2186(6) 0.1998(7) 0.8166(4) 0.0379(18) Uani d . 1 1 H H1 0.2344 0.2904 0.7674 0.045 Uiso calc R 1 1 H H2 0.2535 0.2157 0.9110 0.045 Uiso calc R 1 1 H H3 0.0682 0.1653 0.8086 0.045 Uiso calc R 1 1 O O1 0.7997(6) 0.0222(7) 0.7566(5) 0.0586(19) Uani d . 1 1 O O2 0.6773(6) 0.2246(7) 0.8853(5) 0.0490(19) Uani d . 1 1 C C1 0.3846(8) 0.0797(9) 0.7544(5) 0.039(2) Uani d . 1 1 H H4 0.3355 -0.0242 0.7919 0.047 Uiso calc R 1 1 O O3 0.4252(7) 0.2288(7) 0.5304(5) 0.0549(19) Uani d . 1 1 H H5 0.3054 0.2693 0.4940 0.066 Uiso calc R 1 1 C C2 0.3647(9) 0.0752(8) 0.5891(6) 0.039(2) Uani d . 1 1 H H6 0.4728 -0.0043 0.5498 0.046 Uiso calc R 1 1 H H7 0.2023 0.0472 0.5608 0.046 Uiso calc R 1 1 C C3 0.6421(9) 0.1090(11) 0.8044(6) 0.043(2) Uani d . 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 N1 0.0312(18) 0.036(7) 0.046(4) 0.000(3) 0.002(2) 0.003(2) O1 0.0348(17) 0.058(7) 0.083(4) 0.004(2) 0.008(2) -0.027(3) O2 0.044(2) 0.043(7) 0.060(4) 0.002(3) -0.012(2) -0.018(2) C1 0.037(2) 0.047(9) 0.034(4) -0.010(4) 0.010(3) -0.001(3) O3 0.056(2) 0.064(7) 0.045(3) 0.006(3) 0.002(2) 0.009(2) C2 0.037(3) 0.040(9) 0.038(5) 0.003(4) -0.009(2) -0.007(3) C3 0.036(3) 0.068(9) 0.025(4) -0.006(4) -0.001(3) -0.001(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 C1 N1 H1 109.5 C1 N1 H2 109.5 H1 N1 H2 109.5 C1 N1 H3 109.5 H1 N1 H3 109.5 H2 N1 H3 109.5 N1 C1 C2 110.5(5) N1 C1 C3 111.3(5) C2 C1 C3 111.7(4) N1 C1 H4 107.7 C2 C1 H4 107.7 C3 C1 H4 107.7 C2 O3 H5 109.5 O3 C2 C1 109.2(5) O3 C2 H6 109.8 C1 C2 H6 109.8 O3 C2 H7 109.8 C1 C2 H7 109.8 H6 C2 H7 108.3 O1 C3 O2 124.7(5) O1 C3 C1 118.2(6) O2 C3 C1 117.0(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C1 1.484(7) N1 H1 0.8900 N1 H2 0.8900 N1 H3 0.8900 O1 C3 1.223(7) O2 C3 1.236(9) C1 C2 1.506(7) C1 C3 1.526(7) C1 H4 0.9800 O3 C2 1.441(8) O3 H5 0.8200 C2 H6 0.9700 C2 H7 0.9700 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 H3 O1 1_455 0.89 1.98 2.827(6) 158.5 N1 H3 O2 1_455 0.89 2.34 3.088(5) 141.5 N1 H2 O2 3_457 0.89 1.97 2.793(6) 154.1 N1 H1 O1 4_656 0.89 1.98 2.802(8) 153.6 O3 H5 O3 3_456 0.82 2.13 2.864(2) 148.8 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 N1 C1 C2 O3 60.0(6) C3 C1 C2 O3 -64.5(6) N1 C1 C3 O1 -177.2(7) C2 C1 C3 O1 -53.1(9) N1 C1 C3 O2 -0.7(10) C2 C1 C3 O2 123.4(8) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 5736