An Exciton-Coupled Circular Dichroism Protocol for the Determination of Identity, Chirality, and Enantiomeric Excess of Chiral Secondary Alcohols
Lei You; Gennaro Pescitelli; Eric V. Anslyn; Lorenzo Di Bari; Journal of the American Chemical Society 134 (2012) 7117–7125; doi:10.1021/ja301252h

data_4117858
_publ_section_title
;
 An Exciton-Coupled Circular Dichroism Protocol for the Determination of
 Identity, Chirality, and Enantiomeric Excess of Chiral Secondary Alcohols
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7117
_journal_page_last               7125
_journal_paper_doi               10.1021/ja301252h
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C22 H24 Cl2 N6 O9 Zn'
_chemical_formula_weight         652.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 108.603(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6293(15)
_cell_length_b                   10.7594(9)
_cell_length_c                   14.4721(13)
_cell_measurement_temperature    100(2)
_cell_volume                     2749.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(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     0.71069
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            55135
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  0.9137
_exptl_absorpt_correction_T_min  0.7392
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00000(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   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          1.747
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+2.5421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                5800
_reflns_number_total             6241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja301252h_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4117858