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_1566852
_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         'C18 H35 Cl N2 O P2'
_chemical_formula_sum            'C18 H35 Cl N2 O P2'
_chemical_formula_weight         392.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                90
_cell_angle_beta                 114.8686(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2116(2)
_cell_length_b                   22.6532(5)
_cell_length_c                   10.5288(2)
_cell_measurement_reflns_used    38732
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2209.74(8)
_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 0.987
_diffrn_measured_fraction_theta_max 0.964
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16786
_diffrn_reflns_point_group_measured_fraction_full 0.856
_diffrn_reflns_point_group_measured_fraction_max 0.798
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.469
_diffrn_reflns_theta_min         3.567
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  1.002
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
Flack x determined using 2428 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8105
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0558P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0940
_reflns_Friedel_coverage         0.615
_reflns_Friedel_fraction_full    0.717
_reflns_Friedel_fraction_max     0.624
_reflns_number_gt                6708
_reflns_number_total             8105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01692c3.cif
_cod_data_source_block           1
_cod_original_cell_volume        2209.73(8)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1566852
_cambridge_user_name             'Andrew Peel'
_cambridge_user_crsid            ajp208
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Peel'
_cambridge_crystallographer_crsid ajp208
_cambridge_sample_id             AJP525A
_cambridge_data_id               DW_K1_0043
_shelx_estimated_absorpt_t_min   0.854
_shelx_estimated_absorpt_t_max   0.895
_shelx_res_checksum              15238
_shelx_hkl_checksum              91637