Selectivity and Enantiomeric Resolution in Inclusion Chemistry: A Systematic Study of Chiral Discrimination through Crystallization
Báthori, Nikoletta B.; Nassimbeni, Luigi R.; Crystal Growth & Design 10 (2010) 1782–; doi:10.1021/cg901461k

data_4502631
_publ_section_title
;
 Selectivity and Enantiomeric Resolution in Inclusion Chemistry: A
 Systematic Study of Chiral Discrimination through Crystallization
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1782
_journal_paper_doi               10.1021/cg901461k
_journal_volume                  10
_journal_year                    2010
_chemical_absolute_configuration rm
_chemical_formula_sum            'C38 H45 N O4'
_chemical_formula_weight         579.75
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.05(3)
_cell_angle_beta                 96.03(3)
_cell_angle_gamma                96.08(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5948(19)
_cell_length_b                   10.023(2)
_cell_length_c                   17.167(3)
_cell_measurement_reflns_used    11499
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.71
_cell_measurement_theta_min      2.58
_cell_volume                     1621.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35711
_diffrn_reflns_theta_full        25.71
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_coef       0.0233(15)
_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   1.083
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         11499
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0395P)^2^+0.9083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1224
_reflns_number_gt                9255
_reflns_number_total             11499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg901461k_si_006.cif
_cod_data_source_block           9_seriesII
_cod_original_cell_volume        1621.1(6)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4502631