Structural differences/similarities of diastereotopic groups in three new chiral phosphoramides
Lal Zakaria, Negin; Pourayoubi, Mehrdad; Eghbali Toularoud, Mahsa; Dušek, Michal; Skorepova, Eliska; Acta Crystallographica Section C 77 (2021) 186–196; doi:10.1107/S2053229621002047

data_2022347
_publ_section_title
;
 Structural differences/similarities of diastereotopic groups in three new
 chiral phosphoramides
;
_journal_coeditor_code           FP3087
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              186
_journal_page_last               196
_journal_paper_doi               10.1107/S2053229621002047
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C25 H28 F2 N3 O2 P1'
_chemical_formula_moiety         'C25 H28 F2 N3 O2 P1'
_chemical_formula_sum            'C25 H28 F2 N3 O2 P'
_chemical_formula_weight         471.49
_chemical_name_systematic
'<i>N</i>-(2,6-Difluorobenzoyl)-<i>N</i>',<i>N</i>''-bis[(<i>R</i>)-(+)-\a-ethylbenzyl]phosphoric triamide'
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.97120(10)
_cell_length_b                   20.1758(2)
_cell_length_c                   22.7451(3)
_cell_measurement_reflns_used    24203
_cell_measurement_temperature    120
_cell_measurement_theta_max      68
_cell_measurement_theta_min      4
_cell_volume                     2281.29(6)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_collection
;
GEMINI (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_molecular_graphics
;
CAMERON (Watkin <i>et al.</i>,  1996)
;
_computing_publication_material
;
CRYSTALS (Betteridge <i>et al.</i>,  2003)
;
_computing_structure_refinement
;
CRYSTALS (Betteridge <i>et al.</i>,  2003)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>, 1994)
;
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_av_unetI/netI     0.073
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46145
_diffrn_reflns_theta_full        67.661
_diffrn_reflns_theta_max         67.661
_diffrn_reflns_theta_min         2.928
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.450
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.593
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.19
_refine_diff_density_min         -0.32
_refine_ls_abs_structure_details
;
Parsons <i>et al.</i> (2013),
1653 Friedel Pairs
;
_refine_ls_abs_structure_Flack   0.007(8)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4088
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.0051084
_refine_ls_shift/su_mean         0.0007296
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 1.67P]
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0781
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                3979
_reflns_number_total             4088
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            fp3087sup1.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C25 H28 F2 N3 O2 P1'
_cod_database_code               2022347
_cod_database_fobs_code          2022347