Supramolecular architectures of succinates of 1-hydroxypropan-2-aminium derivatives
Żesławska, Ewa; Nitek, Wojciech; Marona, Henryk; Waszkielewicz, Anna M.; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618008574

data_2021169
_publ_section_title
;
 Supramolecular architectures of succinates of 1-hydroxypropan-2-aminium
 derivatives
;
_journal_coeditor_code           SK3695
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618008574
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '2C13 H22 N O2 +, C4 H4 O4 2-'
_chemical_formula_moiety         '2(C13 H22 N O2 +), C4 H4 O4 2-'
_chemical_formula_sum            'C30 H48 N2 O8'
_chemical_formula_weight         564.7
_chemical_name_systematic
'Bis{(<i>S</i>)-(+)-<i>N</i>-[2-(2,6-dimethylphenoxy)ethyl]-1-hydroxypropan-2-aminium} succinate'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.0820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.19420(10)
_cell_length_b                   8.61420(10)
_cell_length_c                   31.6661(2)
_cell_measurement_reflns_used    29916
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      71.413
_cell_measurement_theta_min      3.951
_cell_volume                     3049.12(5)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008) and SHELXL2014 (Sheldrick, 2015)
;
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova source diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            41881
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.475
_diffrn_reflns_theta_min         3.955
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.71015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.23
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.657
_exptl_crystal_size_mid          0.477
_exptl_crystal_size_min          0.365
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.311
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 5231 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons & Flack (2004)
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_coef       0.00376(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         11732
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.6161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                11518
_reflns_number_total             11732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3695sup1.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2021169
_cod_database_fobs_code          2021169
_shelx_estimated_absorpt_t_min   0.648
_shelx_estimated_absorpt_t_max   0.778
_shelx_hkl_checksum              41958
_shelx_res_checksum              30862
_shelxl_version_number           .2013