Proton-transfer salts of diphenylphosphinic acid with substituted 2-aminopyridine: crystal structure, spectroscopic and DFT studies.
Yuan, Haokun; Zhang, Ran; Hu, Kai; Fang, Ruiqin; Acta crystallographica. Section C, Structural chemistry 79 (2023) 193–203; doi:10.1107/S2053229623003388

data_2312096
_publ_section_title
;
 Proton-transfer salts of diphenylphosphinic acid with substituted
 2-aminopyridine: crystal structure, spectroscopic and DFT studies.
;
_journal_coeditor_code           DG3040
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              193
_journal_page_last               203
_journal_paper_doi               10.1107/S2053229623003388
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C6 H9 N2 +, C12 H10 O2 P -'
_chemical_formula_moiety         'C6 H9 N2 +, C12 H10 O2 P -'
_chemical_formula_sum            'C18 H19 N2 O2 P'
_chemical_formula_weight         326.32
_chemical_name_systematic
;
2-Amino-5-methylpyridinium diphenylphosphinate
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/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                 97.344(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.998(12)
_cell_length_b                   10.747(5)
_cell_length_c                   11.362(5)
_cell_measurement_reflns_used    2174
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      2.36
_cell_volume                     3391(3)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9017
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.9679
_exptl_absorpt_correction_T_min  0.9564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.354
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0684P)^2^+0.6163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                2333
_reflns_number_total             3330
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            dg3040sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 2312094--2312096.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               2312096
_cod_database_fobs_code          2312096