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_1566869
_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         'C28 H50 N3 O P2 +, I -'
_chemical_formula_sum            'C28 H50 I N3 O P2'
_chemical_formula_weight         633.55
_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-2018/1
_audit_update_record
;
2021-08-26 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.4314(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.98080(10)
_cell_length_b                   28.8020(3)
_cell_length_c                   11.8786(2)
_cell_measurement_reflns_used    57388
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     3220.21(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 0.986
_diffrn_measured_fraction_theta_max 0.971
_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  0.0522
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35917
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         3.552
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
Flack x determined using 3757 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.035(12)
_refine_ls_extinction_coef       0.0032(4)
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         13964
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.953
_reflns_Friedel_fraction_max     0.915
_reflns_number_gt                9679
_reflns_number_total             13964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01692c3.cif
_cod_data_source_block           8R
_cod_original_cell_volume        3220.20(7)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1566869
_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             AJP554A
_cambridge_data_id               DW_K3_0090
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.859
_shelx_res_checksum              45194
_shelx_hkl_checksum              95364