Crystal structure of 1-[(1<i>S</i>,2<i>R</i>)-2-hydroxy-1-methyl-2-phenylethyl]pyrrolidinium 2-amino-5-chlorobenzoate
Li, Yunli; Li, Zhanjun; Hu, Yanjie; Li, Wen; Acta Crystallographica Section E 71 (2015) o584–o585; doi:10.1107/S2056989015013389

data_2240938
_publ_section_title
;
 Crystal structure of
 1-[(1<i>S</i>,2<i>R</i>)-2-hydroxy-1-methyl-2-phenylethyl]pyrrolidinium
 2-amino-5-chlorobenzoate
;
_journal_coeditor_code           HB7464
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o584
_journal_page_last               o585
_journal_paper_doi               10.1107/S2056989015013389
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C13 H20 N O +, C7 H5 Cl N O2 -'
_chemical_formula_moiety         'C13 H20 N O +, C7 H5 Cl N O2 -'
_chemical_formula_sum            'C20 H25 Cl N2 O3'
_chemical_formula_weight         376.87
_chemical_melting_point_gt       402
_chemical_melting_point_lt       404
_chemical_name_systematic
;
1-[(1<i>S</i>,2<i>R</i>)-2-Hydroxy-1-methyl-2-phenylethyl]pyrrolidinium
2-amino-5-chlorobenzoate
;
_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'
_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
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6756(3)
_cell_length_b                   11.5541(3)
_cell_length_c                   15.9228(4)
_cell_measurement_reflns_used    1586
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      71.7
_cell_measurement_theta_min      4.7
_cell_volume                     1964.03(9)
_computing_cell_refinement
;
<i>CrysAlis PRO</i> (Agilent, 2012)
;
_computing_data_collection
;
<i>CrysAlis PRO</i> (Agilent, 2012)
;
_computing_data_reduction
;
<i>CrysAlis PRO</i> (Agilent, 2012)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Agilent Xcalibur Eos Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4968
_diffrn_reflns_theta_full        72.32
_diffrn_reflns_theta_max         72.32
_diffrn_reflns_theta_min         4.73
_exptl_absorpt_coefficient_mu    1.897
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis PRO</i>; Agilent, 2012)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ' '
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.181
_refine_ls_abs_structure_details 'Flack (1983) '
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       0.0019(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.0389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                2805
_reflns_number_total             3173
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7464sup1.cif
_cod_data_source_block           I
_cod_database_code               2240938
_cod_database_fobs_code          2240938