Crystal structure of 1,2,3,4-tetra-hydro-isoquinolin-2-ium (2<i>S</i>,3<i>S</i>)-3-carb-oxy-2,3-di-hydroxy-propano-ate monohydrate.
Seidel, Rüdiger W; Kolev, Tsonko M.; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 763–766; doi:10.1107/S2056989024005711

data_2023174
_publ_section_title
;
 Crystal structure of 1,2,3,4-tetra-hydro-isoquinolin-2-ium
 (2<i>S</i>,3<i>S</i>)-3-carb-oxy-2,3-di-hydroxy-propano-ate monohydrate.
;
_journal_coeditor_code           TX2087
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              763
_journal_page_last               766
_journal_paper_doi               10.1107/S2056989024005711
_journal_volume                  80
_journal_year                    2024
_chemical_absolute_configuration syn
_chemical_formula_iupac          'C9 H12 N +, C4 H5 O6 -, H2 O'
_chemical_formula_moiety         'C9 H12 N +, C4 H5 O6 -, H2 O'
_chemical_formula_sum            'C13 H19 N O7'
_chemical_formula_weight         301.29
_chemical_name_common
;
1,2,3,4-Tetrahydroisoquinolinium D-hydrogen tartrate monohydrate
;
_chemical_name_systematic
;
1,2,3,4-Tetrahydroisoquinolin-2-ium
(2<i>S</i>,3<i>S</i>)-3-carboxy-2,3-dihydroxypropanoate monohydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0695(3)
_cell_length_b                   7.4842(3)
_cell_length_c                   26.9573(10)
_cell_measurement_reflns_used    5780
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.7030
_cell_measurement_theta_min      3.0140
_cell_volume                     1426.30(10)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_data_collection
;
<i>CrysAlis</i> system (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2018)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      115(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            16488
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.463
_diffrn_reflns_theta_min         2.825
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSPACK in CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       prism
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.193
_refine_ls_abs_structure_details
;
 The absolute structure was inferred from the known absolute configuration
of the starting material.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3307
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0326P)^2^+0.2898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                2900
_reflns_number_total             3307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tx2087.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023174.cif.'
_cod_database_code               2023174
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.977
_shelx_hkl_checksum              26216
_shelx_res_checksum              17245