#------------------------------------------------------------------------------ #$Date: 2016-08-07 11:31:16 +0300 (Sun, 07 Aug 2016) $ #$Revision: 185253 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/56/7225616.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_7225616 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 102.337(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.8107(6) _cell_length_b 9.3013(8) _cell_length_c 20.411(3) _cell_measurement_reflns_used 5254 _cell_measurement_temperature 125(2) _cell_measurement_theta_max 29.41 _cell_measurement_theta_min 2.04 _cell_volume 892.22(19) _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 125(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 0.992 _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 0.0483 _diffrn_reflns_av_unetI/netI 0.0485 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.992 _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 -27 _diffrn_reflns_number 7901 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.200 _diffrn_reflns_theta_min 2.043 _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 0.159 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.676 _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 0.285 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.081 _refine_ls_extinction_coef 0.018(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 1.013 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 168 _refine_ls_number_reflns 2412 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0378 _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^)+(0.0580P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.1116 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1516 _reflns_number_total 2412 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6ce00561f17.cif _cod_data_source_block gta125K _cod_depositor_comments 'Adding full bibliography for 7225609--7225638.cif.' _cod_original_cell_volume 892.23(18) _cod_database_code 7225616 _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 0.940 _shelx_estimated_absorpt_t_max 0.983 _shelx_res_file ; D:\IPDS\2014\glytart\cooling\125\deposit\new.res created by SHELXL-2014/7 TITL CELL 0.71073 4.81070 9.30130 20.41130 90.00000 102.33700 90.00000 ZERR 4 0.00060 0.00080 0.00260 0.00000 0.01000 0.00000 LATT 1 SYMM -X, Y+ 0.50000, -Z+ 0.50000 SFAC C H N O UNIT 24 44 4 32 TEMP -148 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 0.058000 EXTI 0.017638 FVAR 0.75879 O6 4 0.761696 0.120266 0.564908 11.00000 0.01345 0.01850 = 0.02167 0.00112 0.00007 -0.00244 H6 2 0.579332 0.132473 0.542922 11.00000 -1.20000 O3 4 0.601294 0.355619 0.432755 11.00000 0.02372 0.01872 = 0.01966 0.00168 -0.00131 0.00306 H3 2 0.458122 0.356970 0.395451 11.00000 -1.20000 O5 4 1.223469 0.145474 0.492759 11.00000 0.01765 0.01975 = 0.02304 -0.00458 0.00099 0.00144 H5 2 1.147989 0.075505 0.470144 11.00000 -1.20000 O8 4 1.221389 0.157430 0.662937 11.00000 0.01976 0.02136 = 0.02038 0.00405 0.00078 -0.00145 O7 4 1.328469 0.364703 0.616694 11.00000 0.02397 0.02130 = 0.02131 0.00173 -0.00291 -0.00775 AFIX 147 H7 2 1.467537 0.365484 0.649547 11.00000 -1.20000 AFIX 0 O4 4 0.748769 0.146386 0.395312 11.00000 0.02107 0.02286 = 0.02059 -0.00374 0.00029 0.00018 O1 4 1.222139 0.587071 0.293480 11.00000 0.01855 0.01772 = 0.02356 -0.00126 -0.00086 -0.00254 C3 1 0.774525 0.247174 0.434705 11.00000 0.01849 0.01683 = 0.01815 0.00282 0.00562 -0.00139 O2 4 1.180835 0.362340 0.331642 11.00000 0.02359 0.02063 = 0.02354 0.00416 -0.00223 0.00081 C5 1 0.917941 0.248151 0.561148 11.00000 0.01573 0.01499 = 0.01870 0.00066 0.00318 -0.00160 H5A 2 0.804272 0.333769 0.563378 11.00000 -1.20000 C2 1 1.098595 0.467773 0.293709 11.00000 0.01697 0.01756 = 0.01656 -0.00290 0.00421 0.00171 C6 1 1.172124 0.250192 0.619971 11.00000 0.01766 0.01563 = 0.01832 -0.00219 0.00555 0.00105 C4 1 1.023409 0.256411 0.494640 11.00000 0.01805 0.01601 = 0.01800 -0.00062 0.00303 -0.00041 H4 2 1.113581 0.347461 0.492704 11.00000 -1.20000 N1 3 0.791787 0.549821 0.187118 11.00000 0.02000 0.01865 = 0.01909 -0.00165 -0.00056 0.00382 H1A 2 0.600386 0.566345 0.163843 11.00000 -1.50000 H1B 2 0.850063 0.636464 0.201761 11.00000 -1.50000 H1C 2 0.898470 0.509965 0.160604 11.00000 -1.50000 C1 1 0.815713 0.449703 0.244926 11.00000 0.01876 0.01784 = 0.01819 -0.00073 0.00288 0.00050 H1D 2 0.661369 0.472572 0.266381 11.00000 -1.20000 H1E 2 0.786621 0.352307 0.227772 11.00000 -1.20000 HKLF 4 REM REM R1 = 0.0378 for 1516 Fo > 4sig(Fo) and 0.0744 for all 2412 data REM 168 parameters refined using 0 restraints END WGHT 0.0580 0.0000 REM Highest difference peak 0.285, deepest hole -0.453, 1-sigma level 0.081 Q1 1 1.1658 0.6430 0.2295 11.00000 0.05 0.29 Q2 1 1.2606 0.4058 0.3495 11.00000 0.05 0.27 Q3 1 1.2483 0.4666 0.6069 11.00000 0.05 0.27 Q4 1 0.7281 0.6682 0.2140 11.00000 0.05 0.27 Q5 1 1.2138 0.6311 0.2734 11.00000 0.05 0.27 Q6 1 0.5811 0.4902 0.3905 11.00000 0.05 0.27 Q7 1 0.9880 0.2656 0.5319 11.00000 0.05 0.27 Q8 1 1.2146 0.1620 0.7204 11.00000 0.05 0.26 Q9 1 1.2187 0.0426 0.7002 11.00000 0.05 0.25 Q10 1 0.7993 0.5505 0.1311 11.00000 0.05 0.25 Q11 1 0.8232 0.0229 0.4374 11.00000 0.05 0.25 Q12 1 1.3197 0.2731 0.4997 11.00000 0.05 0.25 Q13 1 1.2089 0.0625 0.5367 11.00000 0.05 0.25 Q14 1 1.1242 0.0882 0.6505 11.00000 0.05 0.25 Q15 1 0.6200 0.1188 0.4413 11.00000 0.05 0.25 Q16 1 0.4190 0.3072 0.4686 11.00000 0.05 0.24 Q17 1 0.7909 0.1267 0.4592 11.00000 0.05 0.24 Q18 1 1.2486 0.2811 0.5283 11.00000 0.05 0.24 Q19 1 1.2886 0.4911 0.3426 11.00000 0.05 0.24 Q20 1 0.9583 0.1186 0.4812 11.00000 0.05 0.24 Q21 1 0.9269 0.2741 0.5214 11.00000 0.05 0.24 Q22 1 1.1682 0.3637 0.4827 11.00000 0.05 0.23 Q23 1 0.6215 0.5323 0.1204 11.00000 0.05 0.23 Q24 1 0.3656 0.2399 0.5600 11.00000 0.05 0.23 Q25 1 1.5955 0.3633 0.6456 11.00000 0.05 0.23 Q26 1 0.6661 0.3007 0.4336 11.00000 0.05 0.23 Q27 1 1.1303 0.4184 0.3182 11.00000 0.05 0.23 Q28 1 1.2118 0.5596 0.2297 11.00000 0.05 0.23 Q29 1 0.3718 0.5019 0.2286 11.00000 0.05 0.23 Q30 1 1.5871 0.4216 0.6439 11.00000 0.05 0.22 ; _shelx_res_checksum 80452 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 0.7617(3) 0.12027(13) 0.56491(6) 0.0184(3) Uani 1 1 d . . H6 H 0.579(5) 0.132(2) 0.5429(11) 0.022 Uiso 1 1 d . U O3 O 0.6013(3) 0.35562(13) 0.43276(6) 0.0216(3) Uani 1 1 d . . H3 H 0.458(5) 0.357(2) 0.3955(11) 0.026 Uiso 1 1 d . U O5 O 1.2235(3) 0.14547(14) 0.49276(6) 0.0206(3) Uani 1 1 d . . H5 H 1.148(5) 0.076(2) 0.4701(11) 0.025 Uiso 1 1 d . U O8 O 1.2214(3) 0.15743(13) 0.66294(6) 0.0210(3) Uani 1 1 d . . O7 O 1.3285(3) 0.36470(14) 0.61669(6) 0.0233(3) Uani 1 1 d . . H7 H 1.4675 0.3655 0.6495 0.028 Uiso 1 1 calc R U O4 O 0.7488(3) 0.14639(14) 0.39531(6) 0.0221(3) Uani 1 1 d . . O1 O 1.2221(3) 0.58707(13) 0.29348(6) 0.0207(3) Uani 1 1 d . . C3 C 0.7745(4) 0.24717(18) 0.43470(8) 0.0176(4) Uani 1 1 d . . O2 O 1.1808(3) 0.36234(14) 0.33164(6) 0.0237(3) Uani 1 1 d . . C5 C 0.9179(4) 0.24815(18) 0.56115(8) 0.0165(3) Uani 1 1 d . . H5A H 0.804(5) 0.334(2) 0.5634(10) 0.020 Uiso 1 1 d . U C2 C 1.0986(4) 0.46777(18) 0.29371(8) 0.0169(3) Uani 1 1 d . . C6 C 1.1721(4) 0.25019(18) 0.61997(8) 0.0170(4) Uani 1 1 d . . C4 C 1.0234(4) 0.25641(19) 0.49464(8) 0.0175(4) Uani 1 1 d . . H4 H 1.114(5) 0.347(2) 0.4927(10) 0.021 Uiso 1 1 d . U N1 N 0.7918(4) 0.54982(17) 0.18712(8) 0.0200(3) Uani 1 1 d . . H1A H 0.600(5) 0.566(2) 0.1638(11) 0.030 Uiso 1 1 d . U H1B H 0.850(5) 0.636(3) 0.2018(11) 0.030 Uiso 1 1 d . U H1C H 0.898(5) 0.510(2) 0.1606(11) 0.030 Uiso 1 1 d . U C1 C 0.8157(4) 0.44970(19) 0.24493(9) 0.0184(4) Uani 1 1 d . . H1D H 0.661(5) 0.473(2) 0.2664(10) 0.022 Uiso 1 1 d . U H1E H 0.787(5) 0.352(2) 0.2278(11) 0.022 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 0.0134(6) 0.0185(6) 0.0217(6) 0.0011(5) 0.0001(5) -0.0024(5) O3 0.0237(7) 0.0187(6) 0.0197(6) 0.0017(5) -0.0013(5) 0.0031(5) O5 0.0176(6) 0.0197(6) 0.0230(6) -0.0046(5) 0.0010(5) 0.0014(5) O8 0.0198(6) 0.0214(6) 0.0204(6) 0.0040(5) 0.0008(5) -0.0014(5) O7 0.0240(7) 0.0213(6) 0.0213(6) 0.0017(5) -0.0029(5) -0.0077(5) O4 0.0211(7) 0.0229(7) 0.0206(6) -0.0037(5) 0.0003(5) 0.0002(5) O1 0.0185(6) 0.0177(6) 0.0236(7) -0.0013(5) -0.0009(5) -0.0025(5) C3 0.0185(9) 0.0168(8) 0.0181(8) 0.0028(7) 0.0056(7) -0.0014(7) O2 0.0236(7) 0.0206(6) 0.0235(7) 0.0042(5) -0.0022(5) 0.0008(5) C5 0.0157(8) 0.0150(8) 0.0187(8) 0.0007(6) 0.0032(6) -0.0016(7) C2 0.0170(8) 0.0176(8) 0.0166(8) -0.0029(6) 0.0042(7) 0.0017(7) C6 0.0177(9) 0.0156(8) 0.0183(8) -0.0022(7) 0.0056(7) 0.0010(6) C4 0.0181(9) 0.0160(8) 0.0180(8) -0.0006(7) 0.0030(7) -0.0004(7) N1 0.0200(8) 0.0186(8) 0.0191(8) -0.0016(6) -0.0006(6) 0.0038(6) C1 0.0188(8) 0.0178(9) 0.0182(8) -0.0007(7) 0.0029(7) 0.0005(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 109.7(14) C3 O3 H3 113.6(14) C4 O5 H5 111.4(16) C6 O7 H7 109.5 O4 C3 O3 126.75(17) O4 C3 C4 121.58(15) O3 C3 C4 111.67(14) O6 C5 C6 108.30(13) O6 C5 C4 111.45(14) C6 C5 C4 109.44(14) O6 C5 H5A 112.0(12) C6 C5 H5A 108.6(13) C4 C5 H5A 107.0(12) O1 C2 O2 127.00(17) O1 C2 C1 117.00(15) O2 C2 C1 115.97(15) O8 C6 O7 125.87(17) O8 C6 C5 124.08(15) O7 C6 C5 110.04(14) O5 C4 C3 111.08(14) O5 C4 C5 109.82(14) C3 C4 C5 110.68(14) O5 C4 H4 109.1(13) C3 C4 H4 107.6(13) C5 C4 H4 108.5(12) C1 N1 H1A 113.5(13) C1 N1 H1B 109.7(15) H1A N1 H1B 103(2) C1 N1 H1C 105.1(14) H1A N1 H1C 112.3(19) H1B N1 H1C 113(2) N1 C1 C2 111.00(14) N1 C1 H1D 106.6(12) C2 C1 H1D 110.4(13) N1 C1 H1E 108.5(13) C2 C1 H1E 112.4(13) H1D C1 H1E 107.7(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O6 C5 1.418(2) O6 H6 0.90(2) O3 C3 1.304(2) O3 H3 0.91(2) O5 C4 1.417(2) O5 H5 0.83(2) O8 C6 1.217(2) O7 C6 1.314(2) O7 H7 0.8400 O4 C3 1.224(2) O1 C2 1.259(2) C3 C4 1.520(2) O2 C2 1.260(2) C5 C6 1.520(3) C5 C4 1.549(2) C5 H5A 0.97(2) C2 C1 1.514(3) C4 H4 0.96(2) N1 C1 1.488(2) N1 H1A 0.95(2) N1 H1B 0.88(2) N1 H1C 0.90(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 0.90(2) 1.80(2) 2.7016(19) 174(2) 1_455 O3 H3 O2 0.91(2) 1.65(2) 2.5634(19) 175(2) 1_455 O5 H5 O6 0.83(2) 2.04(2) 2.7452(18) 142(2) 3_756 O7 H7 O1 0.84 1.74 2.5579(19) 163.3 3_866 N1 H1C O6 0.90(2) 2.27(2) 2.931(2) 129.6(18) 4_565 N1 H1C O8 0.90(2) 2.19(2) 2.944(2) 140.4(19) 4_565 N1 H1A O4 0.95(2) 1.99(2) 2.921(2) 164(2) 2_655 N1 H1B O2 0.88(2) 2.20(2) 2.939(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 -1.8(2) C4 C5 C6 O8 -123.43(17) O6 C5 C6 O7 177.55(13) C4 C5 C6 O7 55.87(18) O4 C3 C4 O5 6.5(2) O3 C3 C4 O5 -174.54(13) O4 C3 C4 C5 -115.77(17) O3 C3 C4 C5 63.19(18) O6 C5 C4 O5 -65.55(18) C6 C5 C4 O5 54.21(18) O6 C5 C4 C3 57.46(18) C6 C5 C4 C3 177.22(14) O1 C2 C1 N1 23.9(2) O2 C2 C1 N1 -158.05(14)