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_7119506
_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_absolute_configuration ad
_chemical_formula_moiety         'C36 H52 Al2 Li2 N4 O2'
_chemical_formula_sum            'C36 H52 Al2 Li2 N4 O2'
_chemical_formula_weight         640.65
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 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                75.1082(13)
_cell_angle_beta                 77.7169(13)
_cell_angle_gamma                84.5937(13)
_cell_formula_units_Z            2
_cell_length_a                   9.9938(3)
_cell_length_b                   10.2452(3)
_cell_length_c                   19.3556(6)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.70
_cell_measurement_theta_min      2.41
_cell_volume                     1869.74(10)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0310
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55196
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        66.647
_diffrn_reflns_theta_max         66.647
_diffrn_reflns_theta_min         2.409
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
Flack x determined using 5433 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         12837
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0727P)^2^+0.6339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    0.944
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                11917
_reflns_number_total             12837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09671a2.cif
_cod_data_source_block           3SS
_cod_database_code               7119506
_cambridge_user_name             'Raul Garcia-Rodriguez'
_cambridge_user_crsid            rg587
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RG189
_cambridge_data_id               DW_B1_0051
_shelx_estimated_absorpt_t_min   0.823
_shelx_estimated_absorpt_t_max   0.901
_shelx_res_checksum              84535