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_2022346
_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          'C21 H22 N1 O3 P1'
_chemical_formula_moiety         'C21 H22 N1 O3 P1'
_chemical_formula_sum            'C21 H22 N O3 P'
_chemical_formula_weight         367.38
_chemical_melting_point          ?
_chemical_name_systematic
;
Diphenyl [(<i>S</i>)-(-)-\a-4-dimethylbenzylamido]phosphate
;
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           CRYSTALS_ver_14.61_build_6999
_cell_angle_alpha                90
_cell_angle_beta                 96.6380(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.67390(10)
_cell_length_b                   7.27830(10)
_cell_length_c                   22.3071(2)
_cell_measurement_reflns_used    15780
_cell_measurement_temperature    120
_cell_measurement_theta_max      68
_cell_measurement_theta_min      4
_cell_volume                     1882.64(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.035
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21509
_diffrn_reflns_theta_full        67.611
_diffrn_reflns_theta_max         67.611
_diffrn_reflns_theta_min         3.812
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.459
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.996
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.30
_refine_ls_abs_structure_details
;
Parsons <i>et al.</i> (2013),
2934 Friedel Pairs
;
_refine_ls_abs_structure_Flack   -0.021(7)
_refine_ls_extinction_coef       3.6(10)
_refine_ls_extinction_method
;
Larson (1970), Equation 22
;
_refine_ls_goodness_of_fit_ref   0.9842
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6650
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.0001733
_refine_ls_shift/su_mean         0.0000237
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick
 w=1/[\s^2^(F^2^) + ( 0.16P)^2^ + 1.04P]
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1824
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.1824
_reflns_number_gt                6508
_reflns_number_total             6650
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            fp3087sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C21 H22 N1 O3 P1'
_cod_database_code               2022346
_cod_database_fobs_code          2022346