Bis(pyrrolidin-1-yl)phosphinic (2,4-difluorobenzoyl)amide
Keikha, Mojtaba; Pourayoubi, Mehrdad; Jasinski, Jerry P.; Golen, James A.; Acta Crystallographica Section E 68 (2012) o2688–; doi:10.1107/S1600536812034733

data_2236546
_publ_section_title
;
 Bis(pyrrolidin-1-yl)phosphinic (2,4-difluorobenzoyl)amide
;
_journal_coeditor_code           PV2575
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2688
_journal_paper_doi               10.1107/S1600536812034733
_journal_volume                  68
_journal_year                    2012
_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_common
;
(2,4-Difluorobenzoyl)[bis(pyrrolidin-1-yl)phosphoryl]amine
;
_chemical_name_systematic
;
Bis(pyrrolidin-1-yl)phosphinic (2,4-difluorobenzoyl)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                 92.268(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1028(3)
_cell_length_b                   9.9477(2)
_cell_length_c                   18.5465(5)
_cell_measurement_reflns_used    7108
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.33
_cell_measurement_theta_min      3.25
_cell_volume                     1678.11(8)
_computing_cell_refinement
'<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)'
_computing_data_collection
'<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)'
_computing_data_reduction
'<i>CrysAlis RED</i> (Oxford Diffraction, 2010)'
_computing_molecular_graphics    '<i>SHELXTL</i>  (Sheldrick, 2008)'
_computing_publication_material
;
<i>SHELXTL</i>  (Sheldrick, 2008) and <i>enCIFer</i> (Allen <i>et
al.</i>,
2004)
;
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1500
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Eos Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17134
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.9619
_exptl_absorpt_correction_T_min  0.9258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis RED</i>; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.359
_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          0.20
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4339
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.7979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1078
_reflns_number_gt                3828
_reflns_number_total             4339
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pv2575.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2236546
_cod_database_fobs_code          2236546