A non-chiral lithium aluminate reagent for the determination of enantiomeric excess of chiral alcohols.
García-Rodríguez, Raúl; Hanf, Schirin; Bond, Andrew D.; Wright, Dominic S.; Chemical communications (Cambridge, England) 53 (2017) 1225–1228; doi:10.1039/c6cc09671a

data_7119507
_publ_section_title
;
 A non-chiral lithium aluminate reagent for the determination of
 enantiomeric excess of chiral alcohols.
;
_journal_issue                   7
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1225
_journal_page_last               1228
_journal_paper_doi               10.1039/c6cc09671a
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C36 H52 Al2 Li2 N4 O2, 2(C7 H8)'
_chemical_formula_sum            'C50 H68 Al2 Li2 N4 O2'
_chemical_formula_weight         824.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-09-07 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.0610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7021(2)
_cell_length_b                   22.8975(5)
_cell_length_c                   22.1511(5)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.56
_cell_measurement_theta_min      2.78
_cell_volume                     4901.77(18)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            72167
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.732
_diffrn_reflns_theta_max         66.732
_diffrn_reflns_theta_min         2.781
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         8689
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+6.9084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.1951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6706
_reflns_number_total             8689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09671a2.cif
_cod_data_source_block           3RS
_cod_database_code               7119507
_cambridge_user_name             'Raul Garcia-Rodriguez'
_cambridge_user_crsid            rg567
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RG198-racemic
_cambridge_data_id               DW_B1_0054
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.936
_shelx_res_checksum              70496