#------------------------------------------------------------------------------ #$Date: 2016-08-07 11:31:16 +0300 (Sun, 07 Aug 2016) $ #$Revision: 185253 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/56/7225613.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_7225613 loop_ _publ_author_name 'Losev, E. A.' 'Zakharov, B. A.' 'Boldyreva, E. V.' _publ_section_title ; Polymorphic transformations in glycine co-crystals at low temperature and high pressure: two new examples as a follow-up to a glycine--glutaric acid study ; _journal_issue 31 _journal_name_full CrystEngComm _journal_page_first 5869 _journal_paper_doi 10.1039/C6CE00561F _journal_volume 18 _journal_year 2016 _chemical_formula_moiety 'C4 H6 O6, C2 H5 N O2' _chemical_formula_sum 'C6 H11 N O8' _chemical_formula_weight 225.16 _chemical_name_common 'glycine-DL-tartaric acid (1:1)' _chemical_name_systematic 'glycine-DL-tartaric acid (1:1)' _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 mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2016-06-02 deposited with the CCDC. 2016-06-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.850(11) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.8273(7) _cell_length_b 9.3086(9) _cell_length_c 20.535(3) _cell_measurement_reflns_used 4450 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 29.41 _cell_measurement_theta_min 2.00 _cell_volume 899.6(2) _computing_cell_refinement 'STOE X-AREA (Stoe & Cie, 2006)' _computing_data_collection 'STOE X-AREA (Stoe & Cie, 2006)' _computing_data_reduction 'STOE X-RED (Stoe & Cie, 2006)' _computing_molecular_graphics 'Mercury (Macrae et al., 2006)' _computing_publication_material ; Mercury (Macrae et al., 2006), PLATON (Spek, 2009), ; _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 200(2) _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector_type STOE _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_unetI/netI 0.0536 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 7961 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.244 _diffrn_reflns_theta_min 2.034 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_current 30 _diffrn_source_power 1.500 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 0.158 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.662 _exptl_crystal_description block _exptl_crystal_F_000 472 _exptl_crystal_size_max 0.390 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.110 _refine_diff_density_max 0.322 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.071 _refine_ls_extinction_coef 0.021(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 168 _refine_ls_number_reflns 2433 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.939 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0357 _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/[\s^2^(Fo^2^)+(0.0522P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.1034 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1375 _reflns_number_total 2433 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6ce00561f17.cif _cod_data_source_block gta200K _cod_depositor_comments 'Adding full bibliography for 7225609--7225638.cif.' _cod_original_cell_volume 899.7(2) _cod_database_code 7225613 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_estimated_absorpt_t_min 0.941 _shelx_estimated_absorpt_t_max 0.983 _shelx_res_file ; D:\IPDS\2014\glytart\cooling\200\deposit\new.res created by SHELXL-2014/7 TITL CELL 0.71073 4.82730 9.30860 20.53540 90.00000 102.85000 90.00000 ZERR 4 0.00070 0.00090 0.00280 0.00000 0.01100 0.00000 LATT 1 SYMM -X, Y+ 0.50000, -Z+ 0.50000 SFAC C H N O UNIT 24 44 4 32 TEMP -73 EQIV $1 -1+X,+Y,+Z EQIV $2 2-X,-Y,1-Z EQIV $3 3-X,1-Y,1-Z EQIV $4 +X,0.5-Y,-0.5+Z EQIV $5 1-X,0.5+Y,0.5-Z EQIV $6 2-X,0.5+Y,0.5-Z L.S. 20 PLAN 30 SIZE 0.39 0.13 0.11 HTAB O6 O5_$1 HTAB O3 O2_$1 HTAB O5 O6_$2 HTAB O7 O1_$3 HTAB N1 O6_$4 HTAB N1 O8_$4 HTAB N1 O4_$5 HTAB N1 O2_$6 BOND $H CONF MORE -1 FMAP 2 ACTA REM TRANSFORMED TO SPACE GROUP : P21/C:B1 REM TRANSFORMED TO SPACE GROUP : P21/C:B1 REM TRANSFORMED TO SPACE GROUP : P21/N:B2 REM REM REM REM REM REM WGHT 0.052200 EXTI 0.021178 FVAR 0.77314 O6 4 0.760627 0.121006 0.564743 11.00000 0.01702 0.02530 = 0.02922 0.00166 -0.00085 -0.00386 H6 2 0.573399 0.133107 0.543591 11.00000 -1.20000 O3 4 0.597750 0.354858 0.432949 11.00000 0.03227 0.02636 = 0.02726 0.00287 -0.00342 0.00558 H3 2 0.458155 0.360926 0.394500 11.00000 -1.20000 O5 4 1.218936 0.145112 0.493340 11.00000 0.02133 0.02799 = 0.03084 -0.00656 0.00006 0.00185 H5 2 1.145030 0.074062 0.469950 11.00000 -1.20000 O8 4 1.220881 0.159479 0.662605 11.00000 0.02665 0.03214 = 0.02819 0.00706 -0.00149 -0.00424 O7 4 1.326322 0.365649 0.616503 11.00000 0.03278 0.03018 = 0.02918 0.00297 -0.00654 -0.01255 AFIX 147 H7 2 1.464547 0.366983 0.649600 11.00000 -1.20000 AFIX 0 O4 4 0.745566 0.147455 0.395525 11.00000 0.02871 0.03222 = 0.02730 -0.00667 -0.00200 0.00102 O1 4 1.225192 0.585313 0.293131 11.00000 0.02441 0.02516 = 0.03182 -0.00155 -0.00392 -0.00473 C3 1 0.771587 0.247166 0.435054 11.00000 0.02301 0.02261 = 0.02131 0.00334 0.00366 -0.00168 O2 4 1.179972 0.362298 0.331537 11.00000 0.03175 0.02982 = 0.03279 0.00674 -0.00564 0.00105 C5 1 0.916374 0.248692 0.560783 11.00000 0.01920 0.01980 = 0.02414 -0.00067 0.00051 -0.00113 H5A 2 0.801651 0.332845 0.563029 11.00000 -1.20000 C2 1 1.099735 0.467284 0.293455 11.00000 0.02217 0.02311 = 0.02192 -0.00236 0.00333 0.00169 C6 1 1.170590 0.251324 0.619589 11.00000 0.02159 0.02271 = 0.02320 -0.00328 0.00492 -0.00131 C4 1 1.019725 0.256192 0.494983 11.00000 0.02202 0.02074 = 0.02476 -0.00051 0.00137 -0.00131 H4 2 1.112390 0.347581 0.493312 11.00000 -1.20000 N1 3 0.795030 0.548996 0.186890 11.00000 0.02657 0.02621 = 0.02489 -0.00267 -0.00457 0.00544 H1A 2 0.607221 0.566032 0.163344 11.00000 -1.50000 H1B 2 0.857673 0.635299 0.201211 11.00000 -1.50000 H1C 2 0.896962 0.507886 0.159069 11.00000 -1.50000 C1 1 0.817505 0.449850 0.244306 11.00000 0.02112 0.02688 = 0.02525 -0.00218 0.00138 0.00006 H1D 2 0.664389 0.474616 0.265234 11.00000 -1.20000 H1E 2 0.786696 0.352460 0.226807 11.00000 -1.20000 HKLF 4 REM REM R1 = 0.0357 for 1375 Fo > 4sig(Fo) and 0.0839 for all 2433 data REM 168 parameters refined using 0 restraints END WGHT 0.0522 0.0000 REM Highest difference peak 0.322, deepest hole -0.333, 1-sigma level 0.071 Q1 1 1.2875 0.6386 0.3228 11.00000 0.05 0.32 Q2 1 1.1833 0.6384 0.2811 11.00000 0.05 0.29 Q3 1 1.2255 0.3606 0.3048 11.00000 0.05 0.26 Q4 1 1.5758 0.4152 0.6459 11.00000 0.05 0.25 Q5 1 1.1699 0.3637 0.4871 11.00000 0.05 0.25 Q6 1 0.9476 0.1479 0.6621 11.00000 0.05 0.24 Q7 1 1.2884 0.5028 0.5816 11.00000 0.05 0.23 Q8 1 1.2524 0.4112 0.3517 11.00000 0.05 0.23 Q9 1 1.2382 0.0274 0.5264 11.00000 0.05 0.22 Q10 1 1.0867 0.2187 0.5029 11.00000 0.05 0.22 Q11 1 1.3519 0.7015 0.2907 11.00000 0.05 0.22 Q12 1 0.8022 0.0953 0.4564 11.00000 0.05 0.22 Q13 1 1.2047 0.4640 0.6188 11.00000 0.05 0.22 Q14 1 1.1070 0.2924 0.5012 11.00000 0.05 0.22 Q15 1 1.3272 0.3235 0.5772 11.00000 0.05 0.22 Q16 1 0.6772 0.1423 0.4223 11.00000 0.05 0.22 Q17 1 1.4578 0.5042 0.3103 11.00000 0.05 0.22 Q18 1 1.1207 0.6846 0.3125 11.00000 0.05 0.21 Q19 1 0.9992 0.2944 0.4634 11.00000 0.05 0.21 Q20 1 0.9557 0.1212 0.4869 11.00000 0.05 0.21 Q21 1 0.7925 0.2361 0.2070 11.00000 0.05 0.21 Q22 1 1.1246 0.4585 0.5785 11.00000 0.05 0.21 Q23 1 0.7671 0.7647 0.2121 11.00000 0.05 0.21 Q24 1 0.6673 0.2112 0.3704 11.00000 0.05 0.21 Q25 1 0.6659 0.1211 0.6027 11.00000 0.05 0.21 Q26 1 1.2798 0.4950 0.3471 11.00000 0.05 0.21 Q27 1 0.8314 0.5013 0.1012 11.00000 0.05 0.20 Q28 1 0.6561 0.0457 0.6024 11.00000 0.05 0.20 Q29 1 0.9876 0.0626 0.4077 11.00000 0.05 0.20 Q30 1 0.9895 0.2589 0.5326 11.00000 0.05 0.20 ; _shelx_res_checksum 660 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 O6 O 0.7606(3) 0.12101(13) 0.56474(6) 0.0248(3) Uani 1 1 d . . H6 H 0.573(5) 0.133(2) 0.5436(10) 0.030 Uiso 1 1 d . U O3 O 0.5977(3) 0.35486(14) 0.43295(7) 0.0302(3) Uani 1 1 d . . H3 H 0.458(5) 0.361(2) 0.3945(11) 0.036 Uiso 1 1 d . U O5 O 1.2189(3) 0.14511(14) 0.49334(7) 0.0276(3) Uani 1 1 d . . H5 H 1.145(5) 0.074(2) 0.4700(11) 0.033 Uiso 1 1 d . U O8 O 1.2209(3) 0.15948(14) 0.66260(6) 0.0302(3) Uani 1 1 d . . O7 O 1.3263(3) 0.36565(14) 0.61650(7) 0.0328(3) Uani 1 1 d . . H7 H 1.4645 0.3670 0.6496 0.039 Uiso 1 1 calc R U O4 O 0.7456(3) 0.14746(14) 0.39553(6) 0.0307(3) Uani 1 1 d . . O1 O 1.2252(3) 0.58531(13) 0.29313(6) 0.0287(3) Uani 1 1 d . . C3 C 0.7716(4) 0.24717(18) 0.43505(8) 0.0225(4) Uani 1 1 d . . O2 O 1.1800(3) 0.36230(14) 0.33154(7) 0.0334(3) Uani 1 1 d . . C5 C 0.9164(4) 0.24869(19) 0.56078(8) 0.0217(4) Uani 1 1 d . . H5A H 0.802(4) 0.333(2) 0.5630(9) 0.026 Uiso 1 1 d . U C2 C 1.0997(4) 0.46728(18) 0.29346(8) 0.0226(4) Uani 1 1 d . . C6 C 1.1706(4) 0.25132(18) 0.61959(8) 0.0225(4) Uani 1 1 d . . C4 C 1.0197(4) 0.25619(19) 0.49498(9) 0.0231(4) Uani 1 1 d . . H4 H 1.112(4) 0.348(2) 0.4933(10) 0.028 Uiso 1 1 d . U N1 N 0.7950(4) 0.54900(18) 0.18689(8) 0.0275(4) Uani 1 1 d . . H1A H 0.607(5) 0.566(2) 0.1633(11) 0.041 Uiso 1 1 d . U H1B H 0.858(5) 0.635(3) 0.2012(11) 0.041 Uiso 1 1 d . U H1C H 0.897(5) 0.508(2) 0.1591(11) 0.041 Uiso 1 1 d . U C1 C 0.8175(4) 0.4498(2) 0.24431(9) 0.0250(4) Uani 1 1 d . . H1D H 0.664(4) 0.475(2) 0.2652(10) 0.030 Uiso 1 1 d . U H1E H 0.787(4) 0.352(2) 0.2268(10) 0.030 Uiso 1 1 d . 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 O6 0.0170(6) 0.0253(7) 0.0292(7) 0.0017(5) -0.0009(5) -0.0039(5) O3 0.0323(8) 0.0264(7) 0.0273(7) 0.0029(6) -0.0034(6) 0.0056(6) O5 0.0213(7) 0.0280(7) 0.0308(7) -0.0066(6) 0.0001(5) 0.0019(5) O8 0.0266(7) 0.0321(7) 0.0282(7) 0.0071(6) -0.0015(5) -0.0042(6) O7 0.0328(8) 0.0302(7) 0.0292(7) 0.0030(6) -0.0065(6) -0.0125(6) O4 0.0287(7) 0.0322(7) 0.0273(7) -0.0067(6) -0.0020(6) 0.0010(6) O1 0.0244(7) 0.0252(6) 0.0318(7) -0.0015(5) -0.0039(5) -0.0047(5) C3 0.0230(9) 0.0226(8) 0.0213(8) 0.0033(7) 0.0037(7) -0.0017(7) O2 0.0317(7) 0.0298(7) 0.0328(7) 0.0067(6) -0.0056(6) 0.0011(6) C5 0.0192(8) 0.0198(8) 0.0241(8) -0.0007(7) 0.0005(7) -0.0011(7) C2 0.0222(8) 0.0231(8) 0.0219(8) -0.0024(7) 0.0033(7) 0.0017(7) C6 0.0216(9) 0.0227(8) 0.0232(8) -0.0033(7) 0.0049(7) -0.0013(7) C4 0.0220(9) 0.0207(8) 0.0248(8) -0.0005(7) 0.0014(7) -0.0013(7) N1 0.0266(9) 0.0262(8) 0.0249(8) -0.0027(6) -0.0046(7) 0.0054(7) C1 0.0211(9) 0.0269(10) 0.0252(9) -0.0022(7) 0.0014(7) 0.0001(7) 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 C5 O6 H6 110.4(13) C3 O3 H3 114.8(13) C4 O5 H5 112.3(15) C6 O7 H7 109.5 O4 C3 O3 126.37(17) O4 C3 C4 121.83(15) O3 C3 C4 111.79(15) O6 C5 C6 108.23(14) O6 C5 C4 111.53(14) C6 C5 C4 109.53(14) O6 C5 H5A 111.1(12) C6 C5 H5A 108.6(12) C4 C5 H5A 107.8(11) O1 C2 O2 126.95(17) O1 C2 C1 117.02(15) O2 C2 C1 116.01(15) O8 C6 O7 125.59(17) O8 C6 C5 124.23(16) O7 C6 C5 110.18(14) O5 C4 C3 110.96(14) O5 C4 C5 109.94(14) C3 C4 C5 110.93(14) O5 C4 H4 108.7(12) C3 C4 H4 108.0(12) C5 C4 H4 108.3(12) C1 N1 H1A 113.9(13) C1 N1 H1B 110.0(15) H1A N1 H1B 104(2) C1 N1 H1C 106.3(14) H1A N1 H1C 109.8(19) H1B N1 H1C 113(2) N1 C1 C2 111.08(15) N1 C1 H1D 106.2(12) C2 C1 H1D 110.1(12) N1 C1 H1E 107.9(12) C2 C1 H1E 112.8(12) H1D C1 H1E 108.6(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O6 C5 1.418(2) O6 H6 0.92(2) O3 C3 1.302(2) O3 H3 0.92(2) O5 C4 1.418(2) O5 H5 0.85(2) O8 C6 1.214(2) O7 C6 1.313(2) O7 H7 0.8400 O4 C3 1.221(2) O1 C2 1.255(2) C3 C4 1.517(2) O2 C2 1.258(2) C5 C6 1.518(2) C5 C4 1.543(2) C5 H5A 0.97(2) C2 C1 1.513(3) C4 H4 0.97(2) N1 C1 1.482(2) N1 H1A 0.94(2) N1 H1B 0.89(2) N1 H1C 0.92(2) C1 H1D 0.96(2) C1 H1E 0.97(2) 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 O6 H6 O5 0.92(2) 1.79(2) 2.7079(18) 172.7(19) 1_455 O3 H3 O2 0.92(2) 1.64(2) 2.5575(19) 172(2) 1_455 O5 H5 O6 0.85(2) 2.04(2) 2.7606(18) 143(2) 3_756 O7 H7 O1 0.84 1.74 2.5597(19) 163.4 3_866 N1 H1C O6 0.92(2) 2.25(2) 2.939(2) 131.7(18) 4_565 N1 H1C O8 0.92(2) 2.20(2) 2.949(2) 138.8(18) 4_565 N1 H1A O4 0.94(2) 2.01(2) 2.924(2) 165(2) 2_655 N1 H1B O2 0.89(2) 2.21(2) 2.947(2) 140(2) 2_755 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 O6 C5 C6 O8 -1.7(2) C4 C5 C6 O8 -123.47(18) O6 C5 C6 O7 177.80(14) C4 C5 C6 O7 56.01(19) O4 C3 C4 O5 6.0(2) O3 C3 C4 O5 -174.97(14) O4 C3 C4 C5 -116.50(18) O3 C3 C4 C5 62.51(18) O6 C5 C4 O5 -65.40(18) C6 C5 C4 O5 54.39(18) O6 C5 C4 C3 57.72(18) C6 C5 C4 C3 177.50(14) O1 C2 C1 N1 23.5(2) O2 C2 C1 N1 -158.21(15)