Stereodynamic Chemosensor with Selective Circular Dichroism and Fluorescence Readout for in Situ Determination of Absolute Configuration, Enantiomeric Excess, and Concentration of Chiral Compounds
Keith W. Bentley; Christian Wolf; Journal of the American Chemical Society 135 (2013) 12200–12203; doi:10.1021/ja406259p

data_4120343
_publ_contact_author             'Christian Wolf'
_publ_contact_author_email       cw27@georgetown.edu
_publ_section_title
;
 Stereodynamic Chemosensor with Selective Circular Dichroism and
 Fluorescence Readout for in Situ Determination of Absolute Configuration,
 Enantiomeric Excess, and Concentration of Chiral Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12200
_journal_page_last               12203
_journal_paper_doi               10.1021/ja406259p
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C36 H28 N2 O3'
_chemical_formula_sum            'C36.75 H29.25 Cl2.25 N2 O3'
_chemical_formula_weight         626.63
_chemical_name_common            '[KB-1]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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                 96.093(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.036(2)
_cell_length_b                   9.7315(16)
_cell_length_c                   44.837(8)
_cell_measurement_reflns_used    10774
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.538
_cell_measurement_theta_min      2.285
_cell_volume                     6089.7(17)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker APEXII'
_computing_molecular_graphics
'ORTEP-3 for Windows; Ferrugia L J (1997), J. Appl. Cryst. 30, 565'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELSL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.1015
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            53449
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         0.91
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS based on Blessing's method; Blessing, Acta Cryst. (1995) A51 33-38'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       plate
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.379
_refine_diff_density_min         -1.624
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1588
_refine_ls_number_reflns         27288
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.0941
_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^)+(0.1101P)^2^+10.9692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2204
_refine_ls_wR_factor_ref         0.2440
_reflns_number_gt                18298
_reflns_number_total             27288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406259p_si_002.cif
_cod_data_source_block           KB-1
_cod_original_cell_volume        6089.8(18)
_cod_database_code               4120343