A pair of diastereomeric 1:2 salts of (<i>R</i>)- and (<i>S</i>)-2-methylpiperazine with (2<i>S</i>,3<i>S</i>)-tartaric acid
Katagiri, Hiroshi; Morimoto, Masao; Sakai, Kenichi; Acta Crystallographica Section C 66 (2010) o20–o24; doi:10.1107/S0108270109046460

data_2017465
_publ_section_title
;
 A pair of diastereomeric 1:2 salts of (<i>R</i>)- and
 (<i>S</i>)-2-methylpiperazine with (2<i>S</i>,3<i>S</i>)-tartaric acid
;
_journal_coeditor_code           EG3031
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o20
_journal_page_last               o24
_journal_paper_doi               10.1107/S0108270109046460
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C5 H14 N2 2+, 2C4 H5 O6 -, H2 O'
_chemical_formula_moiety         'C5 H14 N2 2+, 2(C4 H5 O6 -), H2 O'
_chemical_formula_sum            'C13 H26 N2 O13'
_chemical_formula_weight         418.36
_chemical_name_systematic
;
(<i>S</i>)-2-methylpiperazinediium
bis[hydrogen (2<i>S</i>,3<i>S</i>)-tartrate] monohydrate
;
_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                   7.6062(3)
_cell_length_b                   7.6426(3)
_cell_length_c                   30.3987(11)
_cell_measurement_reflns_used    26172
_cell_measurement_temperature    103
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      3.0
_cell_volume                     1767.11(12)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2003)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and PLATON (Spek, 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita, 2001; Kabuto <i>et al.</i>,  2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0297
_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       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            27022
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.9586
_exptl_absorpt_correction_T_min  0.9196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.185
_refine_ls_abs_structure_details 'see text'
_refine_ls_extinction_coef       0.0134(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         2342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0421P)^2^+0.7169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                2193
_reflns_number_total             2342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            eg3031.cif
_cod_data_source_block           II
_cod_database_code               2017465
_cod_database_fobs_code          2017465