A chiral phosphazane reagent strategy for the determination of enantiomeric excess of amines
Peel, Andrew J.; Terzopoulos, Alexandros; Jethwa, Rajesh B.; Choudhury, Dipanjana; Niu, Hao-Che; Bond, Andrew D.; Slaughter, Jonathan; Wright, Dominic S.; Chemical Science  (2022) –; doi:10.1039/D2SC01692C

data_1566863
_publ_section_title
;
 A chiral phosphazane reagent strategy for the determination of
 enantiomeric excess of amines
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01692C
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H47 N3 O P2'
_chemical_formula_sum            'C27 H47 N3 O P2'
_chemical_formula_weight         491.61
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-08-26 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                103.719(2)
_cell_angle_beta                 90.305(2)
_cell_angle_gamma                94.423(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5547(3)
_cell_length_b                   11.9843(4)
_cell_length_c                   13.3167(4)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.76
_cell_measurement_theta_min      3.42
_cell_volume                     1476.49(8)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-III'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24926
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        66.759
_diffrn_reflns_theta_max         66.759
_diffrn_reflns_theta_min         3.417
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_description       plate
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
Flack x determined using 3669 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.032(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         9670
_refine_ls_number_restraints     477
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0562
_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^)+(0.1178P)^2^+0.2787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1649
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_full    0.848
_reflns_Friedel_fraction_max     0.848
_reflns_number_gt                8828
_reflns_number_total             9670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01692c3.cif
_cod_data_source_block           7S
_cod_database_code               1566863
_cambridge_user_name             'Andrew Peel'
_cambridge_user_crsid            ajp208
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             AJP559B
_cambridge_data_id               DW_B2_0300
_shelx_estimated_absorpt_t_min   0.734
_shelx_estimated_absorpt_t_max   0.929
_shelx_res_checksum              45498
_shelx_hkl_checksum              23174