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_7106017
_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_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 102.557(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   10.381(3)
_cell_length_b                   18.456(5)
_cell_length_c                   19.036(5)
_cell_measurement_reflns_used    14587
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.58
_cell_measurement_theta_min      2.01
_cell_volume                     3559.9(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42152
_diffrn_reflns_theta_full        26.58
_diffrn_reflns_theta_max         26.58
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9842
_exptl_absorpt_correction_T_min  0.9688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0030(4)
_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   1.035
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         14587
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          1.118
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+1.4696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                12252
_reflns_number_total             14587
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC04279J.TXT
_cod_data_source_block           3
_cod_original_cell_volume        3559.7(18)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7106017