Chiral bis(mandelato)borate salts for resolution <i>via</i> metathesis crystallization
Wong, Lawrence W.-Y.; Kan, Jack W.-H.; Sung, Herman H.-Y.; Williams, Ian D.; Acta Crystallographica Section C 73 (2017) –; doi:10.1107/S2053229617009718

data_2020759
_publ_section_title
;
 Chiral bis(mandelato)borate salts for resolution <i>via</i> metathesis
 crystallization
;
_journal_coeditor_code           FM3050
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229617009718
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'N H4 +, C16 H12 B O6 -'
_chemical_formula_moiety         'H4 N +, C16 H12 B O6 -'
_chemical_formula_sum            'C16 H16 B N O6'
_chemical_formula_weight         329.11
_chemical_name_systematic
;
Ammonium bis[(<i>R</i>)-mandelato]borate
;
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.8753(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.49015(16)
_cell_length_b                   8.24219(13)
_cell_length_c                   13.2750(3)
_cell_measurement_reflns_used    2730
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.3210
_cell_measurement_theta_min      5.9280
_cell_volume                     818.50(3)
_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
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector_area_resol_mean 10.3577
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type
'Rigaku SuperNova Dual Source diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4618
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         75.448
_diffrn_reflns_theta_min         3.333
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.138
_refine_diff_density_min         -0.142
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1334 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.12(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3190
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0320P)^2^+0.0440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                3075
_reflns_number_total             3190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fm3050sup1.cif
_cod_data_source_block           jack336a
_cod_database_code               2020759
_cod_database_fobs_code          2020759
_shelx_hkl_checksum              97129
_shelx_res_checksum              83818