Synthesis, Spectroscopic Study and Crystal Structure of a New Single-Enantiomer C(O)NHP(O)-based Phosphoric Triamide, CCl<sub>3</sub>C(O)NHP(O)[(R)-(+)-NHCH(CH<sub>3</sub>)(C<sub>6</sub>H<sub>5</sub>)]<sub>2</sub>·0.25H<sub>2</sub>O
ARIANI, Maral; POURAYOUBI, Mehrdad; DUŠEK, Michal; VAHDANI ALVIRI, Banafsheh; EIGNER, Václav; DAMODARAN, Krishnan; X-ray Structure Analysis Online 33 (2017) 17–; doi:10.2116/xraystruct.33.17

data_1551593
_publ_section_title
;
 Synthesis, Spectroscopic Study and Crystal Structure of a New
 Single-Enantiomer C(O)NHP(O)-based Phosphoric Triamide,
 CCl&lt;sub&gt;3&lt;/sub&gt;C(O)NHP(O)[(R)-(+)-NHCH(CH&lt;sub&gt;3&lt;/sub&gt;)(C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;5&lt;/sub&gt;)]&lt;sub&gt;2&lt;/sub&gt;&#x00B7;0.25H&lt;sub&gt;2&lt;/sub&gt;O
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              17
_journal_paper_doi               10.2116/xraystruct.33.17
_journal_volume                  33
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H21 Cl3 N3 O2 P, 0.203(O)'
_chemical_formula_sum            'C18 H21 Cl3 N3 O2.202 P'
_chemical_formula_weight         451.9
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_cell_angle_alpha                83.6336(17)
_cell_angle_beta                 89.3963(15)
_cell_angle_gamma                73.819(2)
_cell_formula_units_Z            4
_cell_length_a                   9.6898(2)
_cell_length_b                   10.4576(3)
_cell_length_c                   21.0199(3)
_cell_measurement_reflns_used    21686
_cell_measurement_temperature    119.98(10)
_cell_measurement_theta_max      67.15
_cell_measurement_theta_min      4.69
_cell_volume                     2032.53(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_diffrn_ambient_temperature      119.98
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1783
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47594
_diffrn_reflns_theta_full        67.2
_diffrn_reflns_theta_max         67.2
_diffrn_reflns_theta_min         4.23
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.003
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
   CrysAlisPro, Agilent Technologies, Version 1.171.38.41
   Empirical absorption correction using spherical harmonics
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.4769
_exptl_crystal_description       prism
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.552
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.65
_refine_diff_density_min         -0.49
_refine_ls_abs_structure_details
'  6700 of Friedel pairs used in the refinement'
_refine_ls_abs_structure_Flack   0.031(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    2.02
_refine_ls_goodness_of_fit_ref   1.90
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    245
_refine_ls_number_parameters     900
_refine_ls_number_reflns         13943
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.0298
_refine_ls_shift/su_mean         0.0018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0016I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                11230
_reflns_number_total             13943
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            33_17_1.txt
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/andrius/struct/COD-crude-data/automatic-downloads/current/J-STAGE/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 6524 2018-11-02 12:15:13Z antanas 
;
_cod_original_formula_sum        'C18 H21 Cl3 N3 O2.202 P1'
_cod_database_code               1551593