<i>N</i>,<i>N</i>'-Dimethyl-<i>N</i>''-(trichloroacetyl)phosphoramide
Ovchynnikov, Vladimir; Acta Crystallographica Section E 69 (2013) o1759–; doi:10.1107/S1600536813030389

data_2238831
_publ_section_title
;
 <i>N</i>,<i>N</i>'-Dimethyl-<i>N</i>''-(trichloroacetyl)phosphoramide
;
_journal_coeditor_code           BG2520
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1759
_journal_paper_doi               10.1107/S1600536813030389
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C4 H9 Cl3 N3 O2 P'
_chemical_formula_moiety         'C4 H9 Cl3 N3 O2 P'
_chemical_formula_sum            'C4 H9 Cl3 N3 O2 P'
_chemical_formula_weight         268.46
_chemical_name_systematic
;
<i>N</i>,<i>N</i>'-Dimethyl-<i>N</i>''-(trichloroacetyl)phosphoramide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.27(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.231(2)
_cell_length_b                   8.754(2)
_cell_length_c                   12.826(3)
_cell_measurement_reflns_used    2348
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.03
_cell_volume                     1126.6(4)
_computing_cell_refinement
;
<i>CAD-4 EXPRESS</i> (Enraf--Nonius, 1995)
;
_computing_data_collection
;
<i>CAD-4 EXPRESS</i> (Enraf--Nonius, 1995)
;
_computing_data_reduction
;
<i>XCAD4</i> (Harms & Wocadlo, 1996)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/\Q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3806
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.768
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         1908
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1369P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.1954
_reflns_number_gt                1419
_reflns_number_total             1908
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg2520.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2238831