<i>N</i>-(2,6-Difluorobenzoyl)-<i>P</i>,<i>P</i>-bis(pyrrolidin-1-yl)phosphinic amide
Pourayoubi, Mehrdad; Tarahhomi, Atekeh; Rheingold, Arnold L.; Golen, James A.; Acta Crystallographica Section E 67 (2011) o2444–; doi:10.1107/S1600536811033216

data_2231576
_publ_section_title
;
 <i>N</i>-(2,6-Difluorobenzoyl)-<i>P</i>,<i>P</i>-bis(pyrrolidin-1-yl)phosphinic
 amide
;
_journal_coeditor_code           JJ2098
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2444
_journal_paper_doi               10.1107/S1600536811033216
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C15 H20 F2 N3 O2 P'
_chemical_formula_moiety         'C15 H20 F2 N3 O2 P'
_chemical_formula_sum            'C15 H20 F2 N3 O2 P'
_chemical_formula_weight         343.31
_chemical_name_systematic
;
<i>N</i>-(2,6-Difluorobenzoyl)-<i>P</i>,<i>P</i>-bis(pyrrolidin-1-yl)phosphinic
amide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.296(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.286(3)
_cell_length_b                   14.873(4)
_cell_length_c                   10.917(3)
_cell_measurement_reflns_used    7152
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.52
_cell_volume                     1648.2(8)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and enCIFer (Allen <i>et al.</i>, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13279
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.9518
_exptl_absorpt_correction_T_min  0.9245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.410
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3776
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0419P)^2^+1.0825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                2953
_reflns_number_total             3776
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jj2098.cif
_cod_data_source_block           I
_cod_original_cell_volume        1648.3(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2231576
_cod_database_fobs_code          2231576