Crystal structures of two formamidinium hexa-fluorido-phosphate salts, one with batch-dependent disorder.
Neary, Michelle C.; Corfield, Peter W. R.; Parkin, Sean R.; Saba, Shahrokh; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 88–93; doi:10.1107/S2056989023010848

data_2022990
_publ_section_title
;
 Crystal structures of two formamidinium hexa-fluorido-phosphate salts,
 one with batch-dependent disorder.
;
_journal_issue                   'Pt 1'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              88
_journal_page_last               93
_journal_paper_doi               10.1107/S2056989023010848
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C5 H11 N2 +, P F6 -'
_chemical_formula_moiety         'C5 H11 N2 +, F6 P -'
_chemical_formula_sum            'C5 H11 F6 N2 P'
_chemical_formula_weight         244.13
_chemical_name_systematic
;
Pyrrolidinoformamidinium hexafluorophosphate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 105.4000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3588(3)
_cell_length_b                   12.7942(3)
_cell_length_c                   12.2759(3)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      74.50
_cell_measurement_theta_min      3.73
_cell_volume                     1871.38(8)
_computing_cell_refinement
;
SAINT (Bruker, 2022)
;
_computing_data_collection
;
APEX4 (Bruker, 2022)
;
_computing_data_reduction
;
SAINT (Bruker, 2022)
;
_computing_molecular_graphics
;
<i>XP</i> in <i>SHELXTL</i> (Sheldrick, 2008) and WinGX (Farrugia,
2012)
;
_computing_publication_material
;
<i>SHELX</i> (Sheldrick, 2008) and <i>publCIF</i> (Westrip,
2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker D8 with PHOTON III area detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17935
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.581
_diffrn_reflns_theta_min         5.072
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    3.279
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.346
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.49(4)
_refine_ls_extinction_coef       0.0014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3467
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+2.0200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1345
_reflns_number_gt                3450
_reflns_number_total             3467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5706sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 2022988--2022990.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2022990
_cod_database_fobs_code          2022990
_shelx_estimated_absorpt_t_min   0.546
_shelx_estimated_absorpt_t_max   0.714
_shelx_hkl_checksum              35765
_shelx_res_checksum              73682