A new monohydrated molecular salt of GABA with l-tartaric acid: the structure-forming role of water
Losev, E. A.; Pishchur, D. P.; Boldyreva, E. V.; CrystEngComm 23 (2021) 6086–6092; doi:10.1039/D1CE00470K

data_7243134
_publ_section_title
;
 A new monohydrated molecular salt of GABA with l-tartaric acid: the
 structure-forming role of water
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              6086
_journal_page_last               6092
_journal_paper_doi               10.1039/D1CE00470K
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C4 H5 O6, C4 H10 N O2, H2 O'
_chemical_formula_sum            'C8 H17 N O9'
_chemical_formula_weight         271.22
_chemical_name_common            'GABA-L-tartaric acid (1:1) monohydrate'
_chemical_name_systematic        'GABA-L-tartaric acid (1:1) monohydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-06 deposited with the CCDC.	2021-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.007(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1846(2)
_cell_length_b                   27.8403(8)
_cell_length_c                   7.4558(2)
_cell_measurement_reflns_used    4355
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.0560
_cell_measurement_theta_min      2.9090
_cell_volume                     1213.76(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3457
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   75.00  110.00   1.0000  135.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0467  178.0000 -150.0000 35

  2 omega   64.00  100.00   1.0000  135.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0467  178.0000  120.0000 36

  3 omega  -39.00   52.00   1.0000  135.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0467  -19.0000   30.0000 91

  4 omega  -83.00  -53.00   1.0000  135.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0467 -178.0000  -30.0000 30

  5 omega  -69.00   45.00   1.0000  135.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5155   77.0000  -60.0000 114

  6 omega -109.00   15.00   1.0000  135.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5155  -57.0000  -30.0000 124

  7 omega -116.00   16.00   1.0000  135.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5155  -57.0000   90.0000 132

  8 omega -122.00   11.00   1.0000  135.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5155  -57.0000 -150.0000 133

  9 omega  -80.00    1.00   1.0000  135.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5155   37.0000  -90.0000 81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0323016000
_diffrn_orient_matrix_UB_12      -0.0210651000
_diffrn_orient_matrix_UB_13      0.0558461000
_diffrn_orient_matrix_UB_21      0.0770017000
_diffrn_orient_matrix_UB_22      0.0136929000
_diffrn_orient_matrix_UB_23      0.0736269000
_diffrn_orient_matrix_UB_31      -0.0879611000
_diffrn_orient_matrix_UB_32      0.0042411000
_diffrn_orient_matrix_UB_33      0.0398037000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15413
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.463
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_recrystallization_method 'antisolvent crystallization'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4952
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0386P)^2^+0.2652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4034
_reflns_number_total             4952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00470k11.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 7243134.cif.'
_cod_database_code               7243134
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C8 H15 N1 O8'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
2.b Ternary CH refined with riding coordinates:
 C13(H13A), C12(H12D), C23(H23), C22(H22)
2.c Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C27(H27A,H27B), C16(H16A,H16B), C17(H17A,H17B), C28(H28A,
 H28B), C26(H26A,H26B)
2.d Idealised Me refined as rotating group:
 N11(H11A,H11B,H11C), N12(H12A,H12B,H12C)
2.e Idealised tetrahedral OH refined as rotating group:
 O12(H12), O13(H13), O14(H14), O21(H21), O24(H24), O27(H27), O17(H17), O23(H23A)
;
_shelx_res_checksum              27659
_olex2_exptl_crystal_mounting_method 'MiTiGen microloop, cryo-oil'
_olex2_submission_special_instructions 'No special instructions were received'