Quininium mandelates - Systematic study of chiral discrimination in crystals of diastereomeric salts
Nikoletta B. Bathori; Luigi R. Nassimbeni; Clive L. Oliver; Chem.Commun. 47 (2011) 2670–; doi:10.1039/c0cc04279j

data_7106015
_publ_section_title
;
 Quininium mandelates - Systematic study of chiral discrimination in
 crystals of diastereomeric salts
;
_journal_name_full               Chem.Commun.
_journal_page_first              2670
_journal_paper_doi               10.1039/c0cc04279j
_journal_volume                  47
_journal_year                    2011
_chemical_absolute_configuration rm
_chemical_formula_sum            'C28 H32 N2 O5'
_chemical_formula_weight         476.56
_chemical_name_common            quininium-(S)-mandelate
_chemical_name_systematic
;
quininium-(S)-mandelate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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                   6.5538(19)
_cell_length_b                   12.554(3)
_cell_length_c                   31.974(9)
_cell_measurement_reflns_used    2853
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      2.06
_cell_volume                     2630.7(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            9097
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.9677
_exptl_absorpt_correction_T_min  0.9637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0083(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   1.124
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         2853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0709P)^2^+0.1396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                2263
_reflns_number_total             2853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC04279J.TXT
_cod_data_source_block           1
_cod_original_cell_volume        2630.7(13)
_cod_database_code               7106015