Migrating hydrogen in 2,4,6-triaminopyrimidinium(1+) x hydrogen trioxofluorophosphate(−) x monohydrate/2,4,6-triaminopyrimidinium(2+)1–x trioxofluorophosphate(2–)1–x monohydrate (0.0 < x < 0.73) with changing temperature
Matulková, Irena; Fábry, Jan; Němec, Ivan; Císařová, Ivana; Vaněk, Přemysl; Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials 73 (2017) 1114–; doi:10.1107/S2052520617014007

data_2021913
_publ_section_title
;
 Migrating hydrogen in 2,4,6-triaminopyrimidinium(1+)&#x000D; x&#x000D;
 hydrogen trioxofluorophosphate(&#x2212;)&#x000D; x&#x000D;
 monohydrate/2,4,6-triaminopyrimidinium(2+)1--x&#x000D;
 trioxofluorophosphate(2--)1--x&#x000D; monohydrate (0.0 &lt; x &lt; 0.73)
 with changing temperature
;
_journal_coeditor_code           EB5065SUP1
_journal_issue                   6
_journal_name_full
'Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials'
_journal_page_first              1114
_journal_paper_doi               10.1107/S2052520617014007
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         '(C4 N5 H9) (F O3 P) (H2 O)'
_chemical_formula_sum            'C4 H11 F N5 O4 P'
_chemical_formula_weight         243.1
_chemical_name_systematic
; 
2,4,6-triaminopyrimidinium(2+)
fluorophosphonate(2-) monohydrate
;
_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_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 128.6230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.4273(6)
_cell_length_b                   8.7714(2)
_cell_length_c                   13.7988(7)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.985
_cell_measurement_theta_min      2.552
_cell_volume                     1931.62(12)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2015)'
_computing_data_collection
;
<i>Bruker Instrument Service</i>2 (Bruker, 2015)
;
_computing_data_reduction        <i>SAINT</i>
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2005), 
<i>PLATON</i> (Spek, 2009),
<i>JANA</i>2006
;
_computing_publication_material  <i>JANA</i>2006
_computing_structure_refinement
;
<i>JANA</i>2006 (Pet\<r\'i\<cek <i>et al.</i>, 2014)
;
_computing_structure_solution
;
<i>SIR</i>97 (Burla <i>et al.</i>, 2015)
;
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS plate'
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'I\mS  micro-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10111
_diffrn_reflns_theta_full        30
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         2.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  0.9670
_exptl_absorpt_correction_T_min  0.9090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.6721
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.32
_refine_ls_extinction_coef       6300(1000)
_refine_ls_extinction_method
'B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_gt    2.26
_refine_ls_goodness_of_fit_ref   2.16
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    0
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2789
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.0237
_refine_ls_shift/su_mean         0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0004I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                2477
_reflns_number_total             2789
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            eb5065sup1.cif
_cod_data_source_block           XVI
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/IUCr/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C4 H11 F1 N5 O4 P1'
_cod_database_code               2021913
_diffrn_measurement_detector_type 'PHOTON 100 CMOS'
_geom_extra_table_head_d
;
Table 5. 
Hydrogen bonds with F as an acceptor in trioxofluorophosphate 
and in hydrogen trioxofluorophosphate molecules which were retrieved 
from the Cambridge Crystal Structure Database (Groom <i>et al.</i>, 2016). 
For the search, the H...A non-bonding interval was set as 0.9-2.5 \%A. 
There were no hits for O-H...F hydrogen bonds

;
_geom_table_footnote_d
;
^a^F\'abry <i>et al.</i> (2006<i>a</i>) - room temperature determination; 
^b^F\'abry <i>et al.</i> (2012<i>a</i>);
^c^F\'abry <i>et al.</i> (2012<i>b</i>);
^d^F\'abry <i>et al.</i> (2012<i>c</i>).
;
_geom_extra_table_head_e
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Table 6. 
Incidences of selected molecules with fluorine from the search 
in the Cambridge Crystal Structure Database (Groom <i>et al.</i>, 2016) 
and the number of hits/counts with the D-H...F bond 
(the limits for the non-bonded contacts were set as 0.9-2.5 \%A)
;
_geom_table_footnote_e
;
As to [PF~6~]^-^ anion, the counts 
with O-H...F and N-H...F angles (\%) 
below 100 \% have been discarded, the final number of counts
equalled to 3739 and 1130, respectively.
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