Crystal structure of (1,4-diphenyl-4<i>H</i>-1,2,4-triazol-3-yl)phenylamine difluorophosphate, and a survey of the difluorophosphate anion (PO~2~F~2~^{-^})
Weil, Matthias; Fürst, Markus; Acta Crystallographica Section E 76 (2020) 1003–1006; doi:10.1107/S2056989020006933

data_2243528
_publ_section_title
;
 Crystal structure of
 (1,4-diphenyl-4<i>H</i>-1,2,4-triazol-3-yl)phenylamine difluorophosphate,
 and a survey of the difluorophosphate anion (PO~2~F~2~^{-^})
;
_journal_coeditor_code           PK2629
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1003
_journal_page_last               1006
_journal_paper_doi               10.1107/S2056989020006933
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C20 H17 N4 +, P O2 F2 -'
_chemical_formula_moiety         'C20 H17 N4 +, F2 O2 P -'
_chemical_formula_sum            'C20 H17 F2 N4 O2 P'
_chemical_formula_weight         414.35
_chemical_name_systematic
;
3-Anilino-1,4-diphenyl-1<i>H</i>-1,2,4-triazol-4-ium
difluorophosphate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 102.138(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3811(5)
_cell_length_b                   14.9963(9)
_cell_length_c                   16.9217(10)
_cell_measurement_reflns_used    7088
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.883
_cell_measurement_theta_min      2.463
_cell_volume                     1831.2(2)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
MERCURY (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w- and f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30253
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.966
_diffrn_reflns_theta_min         2.462
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            light-brown
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       bar
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.360
_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     266
_refine_ls_number_reflns         5325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+0.7893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                4077
_reflns_number_total             5325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2629sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243528
_cod_database_fobs_code          2243528
_shelx_estimated_absorpt_t_min   0.908
_shelx_estimated_absorpt_t_max   0.981
_shelx_hkl_checksum              55439
_shelx_res_checksum              64228