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_2022989
_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 O +, P F6 -'
_chemical_formula_moiety         'C5 H11 N2 O +, F6 P -'
_chemical_formula_sum            'C5 H11 F6 N2 O P'
_chemical_formula_weight         260.13
_chemical_name_systematic
;
Morpholinoformamidinium hexafluorophosphate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.4504(14)
_cell_length_b                   13.7170(16)
_cell_length_c                   13.4157(14)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.15
_cell_measurement_theta_min      3.38
_cell_volume                     1923.1(4)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2022)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i> (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      100(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42268
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.130
_diffrn_reflns_theta_min         1.949
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.8559
_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    1.797
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.404
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7300
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+0.2600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0881
_reflns_number_gt                5163
_reflns_number_total             7300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5706sup1.cif
_cod_data_source_block           1recryst
_cod_depositor_comments
'Adding full bibliography for 2022988--2022990.cif.'
_cod_database_code               2022989
_cod_database_fobs_code          2022989
_shelx_estimated_absorpt_t_min   0.919
_shelx_estimated_absorpt_t_max   0.952
_shelx_hkl_checksum              2653
_shelx_res_checksum              69840