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_1566861
_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-2018/1
_audit_update_record
;
2021-08-26 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                103.8986(9)
_cell_angle_beta                 90.8396(8)
_cell_angle_gamma                94.8447(15)
_cell_formula_units_Z            2
_cell_length_a                   9.5482(2)
_cell_length_b                   12.0125(3)
_cell_length_c                   13.2604(4)
_cell_measurement_reflns_used    15151
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1470.17(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15471
_diffrn_reflns_point_group_measured_fraction_full 0.808
_diffrn_reflns_point_group_measured_fraction_max 0.745
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.446
_diffrn_reflns_theta_min         3.850
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
Flack x determined using 2665 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_coef       0.018(4)
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         10018
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0625P)^2^+1.0164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.545
_reflns_Friedel_fraction_full    0.622
_reflns_Friedel_fraction_max     0.526
_reflns_number_gt                8123
_reflns_number_total             10018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01692c3.cif
_cod_data_source_block           7RS
_cod_database_code               1566861
_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             AJP547B
_cambridge_data_id               DW_K3_0084B
_shelx_estimated_absorpt_t_min   0.943
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              24048
_shelx_hkl_checksum              82335