##############################################################################
###                                                                        ###
###           Full Paper (Acta Crystallographica Section C)                ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section C. It conforms to the editorial and technical    #
# requirements of Notes for Authors for Section C, and has been peer         #
# reviewed under the auspices of the IUCr Commission on Journals.            #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.4.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
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data_global
_audit_creation_method     SHELXL-97
_journal_data_validation_number     ?
_journal_date_recd_electronic     2009-01-02
_journal_date_accepted     2009-03-23
_journal_name_full     'Acta Crystallographica, Section C'
_journal_year     2009
_journal_volume     65
_journal_issue      6
_journal_page_first     o261
_journal_page_last     o266
_journal_paper_category     FO
_journal_coeditor_code     TR3053
_publ_contact_author_name     'Ewa Matczak-Jon'
_publ_contact_author_address
; Department of Chemistry
  Wrocław University of Technology
  Wybrzeże Wyspiańskiego 27
  50-370 Wrocław
  Poland
;
_publ_contact_author_email     ewa.matczak-jon@pwr.wroc.pl
_publ_contact_author_fax     '+48 71 328 4330'
_publ_contact_author_phone     '+48 71 320 4134'
_publ_section_title
;
Conformational isomers of the hydrogen
[(5-methyl-2-pyridyl)aminomethylene]diphosphonate trianion in salts with
4-aminopyridine and ammonia
;
loop_
    _publ_author_name
    _publ_author_address
    'Ewa Matczak-Jon'
;
Department of Chemistry
Wrocław University of Technology
Wybrzeże Wyspiańskiego 27
50-370 Wrocław
Poland
;
    'Katarzyna Ślepokura'
;
Faculty of Chemistry
University of Wrocław
14 Joliot-Curie Street
50-383 Wrocław
Poland
;
    'Paweł Kafarski'
;
Department of Chemistry
Wrocław University of Technology
Wybrzeże Wyspiańskiego 27
50-370 Wrocław
Poland
;
    'Izabela Skrzyńska'
;
Department of Chemistry
Wrocław University of Technology
Wybrzeże Wyspiańskiego 27
50-370 Wrocław
Poland
;
    'Marek Jon'
;
Faculty of Chemistry
University of Wrocław
14 Joliot-Curie Street
50-383 Wrocław
Poland
;
data_I
_chemical_name_systematic
;
bis(4-aminopyridinium) hydrogen
[(5-methyl-2-pyridinio)aminomethylene]diphosphonate 2.4-hydrate
;
_chemical_name_common     ?
_chemical_formula_moiety     '2(C5 H7 N2 +), C7 H10 N2 O6 P2 2-, 2.4(H2 O)'
_chemical_formula_sum     'C17 H28.80 N6 O8.40 P2'
_chemical_formula_iupac     '2C5 H7 N2 +, C7 H10 N2 O6 P2 2-, 2.4H2 O'
_chemical_formula_weight     513.60
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'C 2/c'
_symmetry_space_group_name_Hall     '-C 2yc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y, -z+1/2'
    'x+1/2, y+1/2, z'
    '-x+1/2, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y, z-1/2'
    '-x+1/2, -y+1/2, -z'
    'x+1/2, -y+1/2, z-1/2'
_cell_length_a     20.385(3)
_cell_length_b     17.838(3)
_cell_length_c     13.038(3)
_cell_angle_alpha     90.00
_cell_angle_beta     101.89(3)
_cell_angle_gamma     90.00
_cell_volume     4639.3(15)
_cell_formula_units_Z     8
_cell_measurement_reflns_used     27791
_cell_measurement_theta_min     2.78
_cell_measurement_theta_max     36.85
_cell_measurement_temperature     100(2)
_exptl_crystal_description     'block'
_exptl_crystal_colour     'colourless'
_exptl_crystal_size_max     0.30
_exptl_crystal_size_mid     0.25
_exptl_crystal_size_min     0.22
_exptl_crystal_density_diffrn     1.471
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     2160
_exptl_absorpt_coefficient_mu     0.246
_exptl_absorpt_correction_type     none
_exptl_absorpt_process_details     ?
_exptl_absorpt_correction_T_min     ?
_exptl_absorpt_correction_T_max     ?
_exptl_special_details
;
;
_diffrn_ambient_temperature     100(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type
             'KUMA KM-4 CCD κ-geometry diffractometer with Sapphire CCD camera'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     38561
_diffrn_reflns_av_R_equivalents     0.0310
_diffrn_reflns_av_sigmaI/netI     0.0162
_diffrn_reflns_theta_min     2.79
_diffrn_reflns_theta_max     29.99
_diffrn_reflns_theta_full     29.99
_diffrn_measured_fraction_theta_max     0.999
_diffrn_measured_fraction_theta_full     0.999
_diffrn_reflns_limit_h_min     -28
_diffrn_reflns_limit_h_max     26
_diffrn_reflns_limit_k_min     -25
_diffrn_reflns_limit_k_max     24
_diffrn_reflns_limit_l_min     -18
_diffrn_reflns_limit_l_max     18
_diffrn_standards_number     ?
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     ?
_refine_special_details
;
Refinement of F² against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F², conventional
R-factors R are based on F, with F set to zero for
negative F². The threshold expression of F² >
σ(F²) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F² are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger.
;
_reflns_number_total     6761
_reflns_number_gt     5813
_reflns_threshold_expression     >2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0443
_refine_ls_R_factor_gt     0.0365
_refine_ls_wR_factor_gt     0.0974
_refine_ls_wR_factor_ref     0.1034
_refine_ls_goodness_of_fit_ref     1.074
_refine_ls_restrained_S_all     1.074
_refine_ls_number_reflns     6761
_refine_ls_number_parameters     408
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment     mixed
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0589P)²+4.7126P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.87
_refine_diff_density_min     -0.31
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C' 0.0033 0.0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H' 0.0000 0.0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N' 0.0061 0.0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'P' 'P' 0.1023 0.0942
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_cell_refinement     'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_reduction     'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics
  'XP in SHELXTL (Version 5.1; Sheldrick, 2008) and DIAMOND (Brandenburg, 2008)'
_computing_publication_material     'SHELXL97 (Sheldrick, 2008)'
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    P P1 0.572726(14) 0.853491(16) 0.38917(2) 0.01047(7) Uani d . 1 . .
    P P2 0.624629(15) 0.709478(17) 0.52188(2) 0.01201(8) Uani d . 1 . .
    O O1 0.49789(4) 0.84730(5) 0.38165(7) 0.01401(17) Uani d . 1 . .
    O O2 0.61034(4) 0.90121(5) 0.47643(7) 0.01533(17) Uani d . 1 . .
    O O3 0.58766(4) 0.88486(5) 0.28248(7) 0.01370(17) Uani d . 1 . .
    H H3 0.5585(13) 0.8719(14) 0.233(2) 0.048(7) Uiso d . 1 . .
    O O4 0.68939(5) 0.74313(6) 0.58273(7) 0.01919(19) Uani d . 1 . .
    O O5 0.56471(5) 0.72053(5) 0.57299(7) 0.01587(17) Uani d . 1 . .
    O O6 0.63437(5) 0.62714(5) 0.49456(7) 0.01730(18) Uani d . 1 . .
    N N1 0.66866(5) 0.75423(6) 0.35379(8) 0.0146(2) Uani d . 1 . .
    H H2 0.7099(11) 0.7626(12) 0.4021(17) 0.032(5) Uiso d . 1 . .
    N N2 0.73489(6) 0.71722(6) 0.23997(9) 0.0177(2) Uani d . 1 . .
    H H4 0.7700(11) 0.7283(13) 0.2954(18) 0.039(6) Uiso d . 1 . .
    C C1 0.60709(6) 0.75785(7) 0.39428(9) 0.0125(2) Uani d . 1 . .
    H H1 0.5744(9) 0.7262(10) 0.3471(14) 0.018(4) Uiso d . 1 . .
    C C2 0.67293(6) 0.72887(7) 0.25817(9) 0.0147(2) Uani d . 1 . .
    C C3 0.61750(6) 0.71266(7) 0.17598(10) 0.0171(2) Uani d . 1 . .
    H H13 0.5745(10) 0.7223(11) 0.1874(16) 0.026(5) Uiso d . 1 . .
    C C4 0.62886(7) 0.68131(8) 0.08495(10) 0.0198(2) Uani d . 1 . .
    H H14 0.5911(10) 0.6691(12) 0.0312(16) 0.028(5) Uiso d . 1 . .
    C C5 0.69462(7) 0.66725(8) 0.07006(10) 0.0208(3) Uani d . 1 . .
    C C6 0.74574(7) 0.68743(8) 0.14945(11) 0.0210(3) Uani d . 1 . .
    H H16 0.7913(11) 0.6822(12) 0.1449(16) 0.032(5) Uiso d . 1 . .
    C C7 0.70676(9) 0.63073(11) -0.02875(12) 0.0331(4) Uani d . 1 . .
    H H7A 0.7551 0.6249 -0.0242 0.050 Uiso calc R 1 . .
    H H7B 0.6879 0.6622 -0.0892 0.050 Uiso calc R 1 . .
    H H7C 0.6852 0.5814 -0.0370 0.050 Uiso calc R 1 . .
    N N11 0.58576(5) 0.80905(6) 0.73669(9) 0.0172(2) Uani d . 1 . .
    H H11 0.5822(10) 0.7814(12) 0.6804(17) 0.030(5) Uiso d . 1 . .
    N N41 0.56928(6) 0.94455(6) 0.98521(9) 0.0179(2) Uani d . 1 . .
    H H41A 0.5785(10) 0.9921(12) 0.9812(16) 0.029(5) Uiso d . 1 . .
    H H41B 0.5522(10) 0.9245(11) 1.0345(16) 0.027(5) Uiso d . 1 . .
    C C21 0.57266(6) 0.77896(7) 0.82543(10) 0.0171(2) Uani d . 1 . .
    H H21 0.5666(9) 0.7242(11) 0.8251(15) 0.023(4) Uiso d . 1 . .
    C C31 0.56769(6) 0.82215(7) 0.90994(10) 0.0158(2) Uani d . 1 . .
    H H31 0.5554(9) 0.8000(10) 0.9676(14) 0.018(4) Uiso d . 1 . .
    C C41 0.57700(6) 0.90073(7) 0.90509(9) 0.0138(2) Uani d . 1 . .
    C C51 0.59314(6) 0.93035(7) 0.81249(10) 0.0161(2) Uani d . 1 . .
    H H51 0.6003(9) 0.9819(10) 0.8055(13) 0.017(4) Uiso d . 1 . .
    C C61 0.59541(6) 0.88350(7) 0.73004(10) 0.0173(2) Uani d . 1 . .
    H H61 0.6030(9) 0.8989(11) 0.6680(15) 0.023(4) Uiso d . 1 . .
    N N12 0.69054(6) 0.55000(7) 0.66449(9) 0.0200(2) Uani d . 1 . .
    H H12 0.6736(11) 0.5786(13) 0.6054(18) 0.037(6) Uiso d . 1 . .
    N N42 0.75427(6) 0.42119(6) 0.92739(9) 0.0175(2) Uani d . 1 . .
    H H42A 0.7964(10) 0.4171(11) 0.9555(15) 0.025(5) Uiso d . 1 . .
    H H42B 0.7229(11) 0.3946(12) 0.9514(17) 0.034(5) Uiso d . 1 . .
    C C22 0.75551(7) 0.55300(8) 0.71456(11) 0.0201(2) Uani d . 1 . .
    H H22 0.7823(10) 0.5852(12) 0.6842(16) 0.028(5) Uiso d . 1 . .
    C C32 0.77868(6) 0.51158(7) 0.80262(10) 0.0176(2) Uani d . 1 . .
    H H32 0.8244(10) 0.5180(11) 0.8378(15) 0.024(5) Uiso d . 1 . .
    C C42 0.73427(6) 0.46371(7) 0.84276(9) 0.0142(2) Uani d . 1 . .
    C C52 0.66619(6) 0.46324(7) 0.78907(10) 0.0169(2) Uani d . 1 . .
    H H52 0.6344(10) 0.4316(12) 0.8137(15) 0.028(5) Uiso d . 1 . .
    C C62 0.64665(7) 0.50598(8) 0.70180(11) 0.0196(2) Uani d . 1 . .
    H H62 0.6015(10) 0.5058(11) 0.6640(15) 0.027(5) Uiso d . 1 . .
    O O1W 0.48746(7) 0.61202(7) 0.64242(13) 0.0401(3) Uani d D 1 . .
    H H1W 0.4820(14) 0.5688(6) 0.617(2) 0.060 Uiso d D 1 . .
    H H2W 0.5100(13) 0.6397(15) 0.614(2) 0.046(7) Uiso d . 1 . .
    O O2W 0.53022(10) 0.53234(10) 0.43113(15) 0.0459(6) Uani d P 0.803(5) A 1
    H H3W 0.5667(18) 0.560(2) 0.456(3) 0.056(9) Uiso d P 0.803(5) A 1
    O O3W 0.5000 0.62111(13) 0.2500 0.0363(6) Uani d SP 0.803(5) A 1
    H H5W 0.5046(12) 0.5902(15) 0.311(2) 0.022(6) Uiso d P 0.803(5) A 1
    O O20W 0.5119(4) 0.5568(5) 0.3671(8) 0.053(3) Uiso d P 0.197(5) A 2
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    P1 O1 . 1.5124(9) yes
    P1 O2 . 1.4991(10) yes
    P1 O3 . 1.5860(10) yes
    P1 C1 . 1.8403(12) yes
    P2 O4 . 1.5169(10) yes
    P2 O5 . 1.5199(10) yes
    P2 O6 . 1.5339(10) yes
    P2 C1 . 1.8425(13) yes
    N1 C1 . 1.460(2) yes
    N1 C2 . 1.346(2) yes
    N2 C2 . 1.348(2) yes
    N2 C6 . 1.353(2) yes
    O3 H3 . 0.81(3) ?
    N1 H2 . 0.95(2) ?
    N2 H4 . 0.93(2) ?
    C1 H1 . 0.99(2) ?
    C2 C3 . 1.418(2) ?
    C3 C4 . 1.374(2) ?
    C3 H13 . 0.93(2) ?
    C4 C5 . 1.416(2) ?
    C4 H14 . 0.95(2) ?
    C5 C6 . 1.357(2) ?
    C5 C7 . 1.509(2) ?
    C6 H16 . 0.95(2) ?
    C7 H7A . 0.98 ?
    C7 H7B . 0.98 ?
    C7 H7C . 0.98 ?
    N11 C61 . 1.348(2) ?
    N11 C21 . 1.351(2) ?
    N11 H11 . 0.87(2) ?
    N41 C41 . 1.340(2) ?
    N41 H41A . 0.87(2) ?
    N41 H41B . 0.87(2) ?
    C21 C31 . 1.365(2) ?
    C21 H21 . 0.98(2) ?
    C31 C41 . 1.418(2) ?
    C31 H31 . 0.93(2) ?
    C41 C51 . 1.417(2) ?
    C51 C61 . 1.370(2) ?
    C51 H51 . 0.94(2) ?
    C61 H61 . 0.90(2) ?
    N12 C22 . 1.352(2) ?
    N12 C62 . 1.354(2) ?
    N12 H12 . 0.93(2) ?
    N42 C42 . 1.332(2) ?
    N42 H42A . 0.86(2) ?
    N42 H42B . 0.90(2) ?
    C22 C32 . 1.365(2) ?
    C22 H22 . 0.94(2) ?
    C32 C42 . 1.420(2) ?
    C32 H32 . 0.96(2) ?
    C42 C52 . 1.420(2) ?
    C52 C62 . 1.359(2) ?
    C52 H52 . 0.96(2) ?
    C62 H62 . 0.95(2) ?
    O1W H1W . 0.84(2) ?
    O1W H2W . 0.82(3) ?
    O2W H3W . 0.90(4) ?
    O3W H5W . 0.96(3) ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1 P1 O2 . . 116.23(6) yes
    O1 P1 O3 . . 110.02(6) yes
    O2 P1 O3 . . 107.74(5) yes
    O1 P1 C1 . . 107.82(5) yes
    O2 P1 C1 . . 111.56(5) yes
    O3 P1 C1 . . 102.61(5) yes
    O4 P2 O5 . . 114.25(6) yes
    O4 P2 O6 . . 111.10(6) yes
    O5 P2 O6 . . 112.34(5) yes
    O4 P2 C1 . . 105.84(6) yes
    O5 P2 C1 . . 108.13(6) yes
    O6 P2 C1 . . 104.42(5) yes
    C1 N1 C2 . . 125.05(11) yes
    C1 N1 H2 . . 117.5(13) yes
    C2 N1 H2 . . 116.6(13) yes
    P1 C1 P2 . . 117.93(6) yes
    P1 C1 N1 . . 112.16(8) yes
    P2 C1 N1 . . 106.53(8) yes
    P1 O3 H3 . . 110(2) ?
    C2 N2 C6 . . 122.77(12) ?
    C2 N2 H4 . . 115.5(14) ?
    C6 N2 H4 . . 121.6(14) ?
    N1 C1 H1 . . 105.7(10) ?
    P1 C1 H1 . . 107.7(10) ?
    P2 C1 H1 . . 106.0(11) ?
    N1 C2 N2 . . 117.16(11) ?
    N1 C2 C3 . . 125.12(12) ?
    N2 C2 C3 . . 117.72(11) ?
    C4 C3 C2 . . 119.08(12) ?
    C4 C3 H13 . . 122.9(12) ?
    C2 C3 H13 . . 118.0(12) ?
    C3 C4 C5 . . 121.55(12) ?
    C3 C4 H14 . . 118.3(12) ?
    C5 C4 H14 . . 120.2(12) ?
    C6 C5 C4 . . 116.63(12) ?
    C6 C5 C7 . . 122.03(13) ?
    C4 C5 C7 . . 121.33(13) ?
    N2 C6 C5 . . 122.09(13) ?
    N2 C6 H16 . . 115.6(13) ?
    C5 C6 H16 . . 122.3(13) ?
    C5 C7 H7A . . 109.5 ?
    C5 C7 H7B . . 109.5 ?
    H7A C7 H7B . . 109.5 ?
    C5 C7 H7C . . 109.5 ?
    H7A C7 H7C . . 109.5 ?
    H7B C7 H7C . . 109.5 ?
    C61 N11 C21 . . 120.24(11) ?
    C61 N11 H11 . . 119.3(14) ?
    C21 N11 H11 . . 119.8(14) ?
    C41 N41 H41A . . 117.3(14) ?
    C41 N41 H41B . . 117.8(14) ?
    H41A N41 H41B . . 125(2) ?
    N11 C21 C31 . . 121.85(12) ?
    N11 C21 H21 . . 115.9(11) ?
    C31 C21 H21 . . 122.3(11) ?
    C21 C31 C41 . . 119.28(12) ?
    C21 C31 H31 . . 119.4(11) ?
    C41 C31 H31 . . 121.2(11) ?
    N41 C41 C51 . . 122.14(12) ?
    N41 C41 C31 . . 120.26(11) ?
    C51 C41 C31 . . 117.59(11) ?
    C61 C51 C41 . . 119.50(12) ?
    C61 C51 H51 . . 119.3(11) ?
    C41 C51 H51 . . 121.1(11) ?
    N11 C61 C51 . . 121.44(12) ?
    N11 C61 H61 . . 114.5(12) ?
    C51 C61 H61 . . 124.1(12) ?
    C22 N12 C62 . . 120.25(12) ?
    C22 N12 H12 . . 122.6(14) ?
    C62 N12 H12 . . 117.2(14) ?
    C42 N42 H42A . . 120.5(13) ?
    C42 N42 H42B . . 118.0(14) ?
    H42A N42 H42B . . 121(2) ?
    N12 C22 C32 . . 121.30(12) ?
    N12 C22 H22 . . 114.8(12) ?
    C32 C22 H22 . . 123.9(13) ?
    C22 C32 C42 . . 119.92(12) ?
    C22 C32 H32 . . 118.2(12) ?
    C42 C32 H32 . . 121.8(12) ?
    N42 C42 C52 . . 120.43(12) ?
    N42 C42 C32 . . 122.54(12) ?
    C52 C42 C32 . . 117.03(11) ?
    C62 C52 C42 . . 119.83(12) ?
    C62 C52 H52 . . 120.4(12) ?
    C42 C52 H52 . . 119.7(12) ?
    N12 C62 C52 . . 121.64(12) ?
    N12 C62 H62 . . 117.2(12) ?
    C52 C62 H62 . . 121.2(12) ?
    H1W O1W H2W . . 114(3) ?
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    O1 P1 C1 P2 . . . . -82.24(8) yes
    O2 P1 C1 P2 . . . . 46.54(9) yes
    O3 P1 C1 P2 . . . . 161.63(6) yes
    O4 P2 C1 P1 . . . . -76.95(8) yes
    O5 P2 C1 P1 . . . . 45.89(8) yes
    O6 P2 C1 P1 . . . . 165.71(7) yes
    O1 P1 C1 N1 . . . . 153.46(8) yes
    O2 P1 C1 N1 . . . . -77.77(9) yes
    O3 P1 C1 N1 . . . . 37.33(9) yes
    O4 P2 C1 N1 . . . . 50.11(9) yes
    O5 P2 C1 N1 . . . . 172.95(7) yes
    O6 P2 C1 N1 . . . . -67.24(9) yes
    C2 N1 C1 P1 . . . . -102.04(12) yes
    C2 N1 C1 P2 . . . . 127.53(11) yes
    C1 N1 C2 N2 . . . . -168.82(11) yes
    C1 N1 C2 C3 . . . . 10.3(2) yes
    C6 N2 C2 N1 . . . . 175.75(12) ?
    C6 N2 C2 C3 . . . . -3.5(2) ?
    N1 C2 C3 C4 . . . . -174.77(12) ?
    N2 C2 C3 C4 . . . . 4.4(2) ?
    C2 C3 C4 C5 . . . . -2.2(2) ?
    C3 C4 C5 C6 . . . . -1.1(2) ?
    C3 C4 C5 C7 . . . . 178.17(14) ?
    C2 N2 C6 C5 . . . . 0.2(2) ?
    C4 C5 C6 N2 . . . . 2.2(2) ?
    C7 C5 C6 N2 . . . . -177.08(14) ?
    C61 N11 C21 C31 . . . . 1.0(2) ?
    N11 C21 C31 C41 . . . . -0.5(2) ?
    C21 C31 C41 N41 . . . . 176.90(12) ?
    C21 C31 C41 C51 . . . . -1.8(2) ?
    N41 C41 C51 C61 . . . . -175.08(12) ?
    C31 C41 C51 C61 . . . . 3.6(2) ?
    C21 N11 C61 C51 . . . . 0.8(2) ?
    C41 C51 C61 N11 . . . . -3.2(2) ?
    C62 N12 C22 C32 . . . . 0.7(2) ?
    N12 C22 C32 C42 . . . . 0.5(2) ?
    C22 C32 C42 N42 . . . . 178.96(12) ?
    C22 C32 C42 C52 . . . . -1.6(2) ?
    N42 C42 C52 C62 . . . . -178.93(12) ?
    C32 C42 C52 C62 . . . . 1.7(2) ?
    C22 N12 C62 C52 . . . . -0.7(2) ?
    C42 C52 C62 N12 . . . . -0.5(2) ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    O3 H3 O1 2_655 0.81(3) 1.75(3) 2.556(2) 173(3)
    N1 H2 O4 . 0.95(2) 2.50(2) 2.934(2) 108(2)
    N1 H2 O4 7_666 0.95(2) 2.02(2) 2.841(2) 143(2)
    N2 H4 O4 7_666 0.93(2) 1.71(2) 2.599(2) 159(2)
    N11 H11 O5 . 0.87(2) 1.75(2) 2.618(2) 172(2)
    N41 H41A O2 6_576 0.87(2) 2.02(2) 2.885(2) 174(2)
    N41 H41B O1 2_656 0.87(2) 2.14(2) 2.979(2) 161(2)
    N12 H12 O6 . 0.93(2) 1.73(2) 2.658(2) 174(2)
    N42 H42A O2 4_646 0.86(2) 1.95(2) 2.809(2) 176(2)
    N42 H42B O6 6_566 0.90(2) 2.04(2) 2.892(2) 158(2)
    O1W H1W O2W 5_666 0.84(2) 1.910(10)
                                      2.746(2) 176(3)
    O1W H2W O5 . 0.82(3) 1.96(3) 2.763(2) 167(3)
    O2W H3W O6 . 0.90(4) 1.82(4) 2.707(2) 171(3)
    O3W H5W O2W . 0.96(3) 1.86(3) 2.804(2) 170(2)
    C1 H1 O3W . 0.99(2) 2.57(2) 3.544(2) 168(2)
    C3 H13 O3W . 0.93(2) 2.60(2) 3.208(2) 123(2)
    C4 H14 O1W 2_655 0.95(2) 2.69(2) 3.611(2) 163(2)
    C6 H16 N11 7_666 0.95(2) 2.66(2) 3.450(2) 141(2)
    C21 H21 O1W 2_656 0.98(2) 2.36(2) 3.280(2) 154(2)
    C31 H31 O1 2_656 0.93(2) 2.58(2) 3.297(2) 135(2)
    C51 H51 O3 6_576 0.94(2) 2.40(2) 3.319(2) 165(2)
    C61 H61 O2 . 0.90(2) 2.53(2) 3.397(2) 162(2)
    C22 H22 O3 7_666 0.94(2) 2.65(2) 3.376(2) 135(2)
    C52 H52 O6 6_566 0.96(2) 2.58(2) 3.304(2) 132(2)
data_II
_chemical_name_systematic
;
triammonium hydrogen [(5-methyl-2-pyridyl)aminomethylene]diphosphonate
monohydrate
;
_chemical_name_common     ?
_chemical_formula_moiety     '3(N H4 +), C7 H9 N2 O6 P2 3-, H2 O'
_chemical_formula_sum     'C7 H23 N5 O7 P2'
_chemical_formula_iupac     '3N H4 +, C7 H9 N2 O6 P2 3-, H2 O'
_chemical_formula_weight     351.24
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/c'
_symmetry_space_group_name_Hall     '-P 2ybc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y-1/2, z-1/2'
_cell_length_a     17.087(3)
_cell_length_b     6.216(2)
_cell_length_c     15.159(3)
_cell_angle_alpha     90.00
_cell_angle_beta     109.84(3)
_cell_angle_gamma     90.00
_cell_volume     1514.5(6)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     14567
_cell_measurement_theta_min     2.85
_cell_measurement_theta_max     36.74
_cell_measurement_temperature     100(2)
_exptl_crystal_description     'plate'
_exptl_crystal_colour     'colourless'
_exptl_crystal_size_max     0.40
_exptl_crystal_size_mid     0.30
_exptl_crystal_size_min     0.05
_exptl_crystal_density_diffrn     1.540
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     744
_exptl_absorpt_coefficient_mu     0.328
_exptl_absorpt_correction_type     'analytical'
_exptl_absorpt_process_details     '(CrysAlis RED; Oxford Diffraction, 2006)'
_exptl_absorpt_correction_T_min     0.894
_exptl_absorpt_correction_T_max     0.984
_exptl_special_details
;
;
_diffrn_ambient_temperature     100(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type
             'KUMA KM-4 CCD κ-geometry diffractometer with Sapphire CCD camera'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     21075
_diffrn_reflns_av_R_equivalents     0.0279
_diffrn_reflns_av_sigmaI/netI     0.0318
_diffrn_reflns_theta_min     2.86
_diffrn_reflns_theta_max     36.83
_diffrn_reflns_theta_full     30.00
_diffrn_measured_fraction_theta_max     0.893
_diffrn_measured_fraction_theta_full     0.982
_diffrn_reflns_limit_h_min     -26
_diffrn_reflns_limit_h_max     28
_diffrn_reflns_limit_k_min     -10
_diffrn_reflns_limit_k_max     8
_diffrn_reflns_limit_l_min     -25
_diffrn_reflns_limit_l_max     17
_diffrn_standards_number     ?
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     ?
_refine_special_details
;
Refinement of F² against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F², conventional
R-factors R are based on F, with F set to zero for
negative F². The threshold expression of F² >
σ(F²) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F² are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger.
;
_reflns_number_total     6808
_reflns_number_gt     5206
_reflns_threshold_expression     >2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0482
_refine_ls_R_factor_gt     0.0317
_refine_ls_wR_factor_gt     0.0827
_refine_ls_wR_factor_ref     0.0925
_refine_ls_goodness_of_fit_ref     1.064
_refine_ls_restrained_S_all     1.064
_refine_ls_number_reflns     6808
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     refall
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0546P)²+0.1044P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.66
_refine_diff_density_min     -0.33
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C' 0.0033 0.0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H' 0.0000 0.0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N' 0.0061 0.0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'P' 'P' 0.1023 0.0942
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_cell_refinement     'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_reduction     'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics
  'XP in SHELXTL (Version 5.1; Sheldrick, 2008) and DIAMOND (Brandenburg, 2008)'
_computing_publication_material     'SHELXL97 (Sheldrick, 2008)'
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    P P1 0.341365(15) 0.26392(4) 0.201243(16) 0.00812(5) Uani d . 1 . .
    P P2 0.345195(14) 0.31899(4) 0.407376(16) 0.00828(5) Uani d . 1 . .
    O O1 0.42304(4) 0.14209(12) 0.23174(5) 0.01227(13) Uani d . 1 . .
    O O2 0.34803(5) 0.50104(12) 0.18320(5) 0.01345(13) Uani d . 1 . .
    O O3 0.27697(4) 0.14987(12) 0.11306(5) 0.01245(13) Uani d . 1 . .
    H H3 0.2871(13) 0.200(4) 0.0597(15) 0.057(6) Uiso d . 1 . .
    O O4 0.43163(4) 0.22149(12) 0.43485(5) 0.01294(13) Uani d . 1 . .
    O O5 0.34573(4) 0.56480(11) 0.40984(5) 0.01209(12) Uani d . 1 . .
    O O6 0.29515(5) 0.22658(12) 0.46570(5) 0.01318(13) Uani d . 1 . .
    N N1 0.20612(5) 0.34165(13) 0.25093(6) 0.01076(14) Uani d . 1 . .
    H H2 0.2079(10) 0.463(3) 0.2237(11) 0.022(4) Uiso d . 1 . .
    N N2 0.12623(5) 0.02884(14) 0.23686(6) 0.01267(14) Uani d . 1 . .
    C C1 0.28757(6) 0.23283(14) 0.28646(6) 0.00875(14) Uani d . 1 . .
    H H1 0.2767(9) 0.079(2) 0.2879(10) 0.017(3) Uiso d . 1 . .
    C C2 0.13340(6) 0.22849(15) 0.20717(6) 0.01032(15) Uani d . 1 . .
    C C3 0.06779(6) 0.32694(17) 0.13447(7) 0.01346(16) Uani d . 1 . .
    H H13 0.0772(9) 0.465(2) 0.1146(10) 0.015(3) Uiso d . 1 . .
    C C4 -0.00483(6) 0.21245(18) 0.09311(7) 0.01478(17) Uani d . 1 . .
    H H14 -0.0490(9) 0.276(2) 0.0425(10) 0.018(4) Uiso d . 1 . .
    C C5 -0.01379(6) 0.00307(17) 0.12347(7) 0.01391(17) Uani d . 1 . .
    C C6 0.05399(6) -0.07791(17) 0.19519(7) 0.01433(17) Uani d . 1 . .
    H H16 0.0510(9) -0.224(3) 0.2205(10) 0.019(4) Uiso d . 1 . .
    C C7 -0.09195(7) -0.12799(19) 0.08137(8) 0.01776(19) Uani d . 1 . .
    H H7A -0.0819(11) -0.274(3) 0.0922(11) 0.028(4) Uiso d . 1 . .
    H H7B -0.1148(10) -0.112(3) 0.0182(12) 0.028(4) Uiso d . 1 . .
    H H7C -0.1351(10) -0.096(3) 0.1099(11) 0.027(4) Uiso d . 1 . .
    O O1W 0.20391(5) 0.72573(14) 0.09839(6) 0.01815(15) Uani d . 1 . .
    H H1W 0.2482(12) 0.658(3) 0.1238(13) 0.034(5) Uiso d . 1 . .
    H H2W 0.2178(13) 0.859(4) 0.1133(14) 0.050(6) Uiso d . 1 . .
    N N10 0.47082(5) 0.79552(14) 0.37136(6) 0.01251(14) Uani d . 1 . .
    H H1N 0.4288(10) 0.707(3) 0.3690(11) 0.020(4) Uiso d . 1 . .
    H H2N 0.4942(10) 0.741(3) 0.3331(11) 0.024(4) Uiso d . 1 . .
    H H3N 0.4521(12) 0.919(3) 0.3513(13) 0.035(5) Uiso d . 1 . .
    H H4N 0.5017(10) 0.803(3) 0.4326(12) 0.028(4) Uiso d . 1 . .
    N N20 0.57577(5) 0.30123(14) 0.39476(6) 0.01189(14) Uani d . 1 . .
    H H5N 0.5238(10) 0.275(2) 0.3928(10) 0.019(4) Uiso d . 1 . .
    H H6N 0.6041(9) 0.338(2) 0.4535(11) 0.017(3) Uiso d . 1 . .
    H H7N 0.5745(10) 0.407(3) 0.3560(11) 0.025(4) Uiso d . 1 . .
    H H8N 0.5955(11) 0.187(3) 0.3767(12) 0.031(4) Uiso d . 1 . .
    N N30 0.22178(6) -0.16098(15) 0.41713(6) 0.01423(15) Uani d . 1 . .
    H H9N 0.2511(10) -0.044(3) 0.4386(11) 0.029(4) Uiso d . 1 . .
    H H10N 0.1831(10) -0.128(3) 0.3594(11) 0.024(4) Uiso d . 1 . .
    H H11N 0.2574(10) -0.264(3) 0.4123(11) 0.026(4) Uiso d . 1 . .
    H H12N 0.1993(11) -0.203(3) 0.4567(12) 0.030(4) Uiso d . 1 . .
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    P1 O1 . 1.5155(8) yes
    P1 O2 . 1.5105(9) yes
    P1 O3 . 1.5817(9) yes
    P1 C1 . 1.8320(10)
                     yes
    P2 O4 . 1.5181(8) yes
    P2 O5 . 1.5284(9) yes
    P2 O6 . 1.5350(8) yes
    P2 C1 . 1.8410(10)
                     yes
    N1 C1 . 1.475(2) yes
    N1 C2 . 1.385(2) yes
    N2 C2 . 1.340(2) yes
    N2 C6 . 1.354(2) yes
    O3 H3 . 0.94(2) ?
    N1 H2 . 0.86(2) ?
    C1 H1 . 0.98(2) ?
    C2 C3 . 1.417(2) ?
    C3 C4 . 1.382(2) ?
    C3 H13 . 0.94(2) ?
    C4 C5 . 1.406(2) ?
    C4 H14 . 0.96(2) ?
    C5 C6 . 1.386(2) ?
    C5 C7 . 1.509(2) ?
    C6 H16 . 1.00(2) ?
    C7 H7A . 0.93(2) ?
    C7 H7B . 0.91(2) ?
    C7 H7C . 0.99(2) ?
    O1W H1W . 0.84(2) ?
    O1W H2W . 0.87(2) ?
    N10 H1N . 0.90(2) ?
    N10 H2N . 0.88(2) ?
    N10 H3N . 0.84(2) ?
    N10 H4N . 0.90(2) ?
    N20 H5N . 0.89(2) ?
    N20 H6N . 0.89(2) ?
    N20 H7N . 0.88(2) ?
    N20 H8N . 0.87(2) ?
    N30 H9N . 0.88(2) ?
    N30 H10N . 0.92(2) ?
    N30 H11N . 0.90(2) ?
    N30 H12N . 0.86(2) ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1 P1 O2 . . 115.13(4) yes
    O1 P1 O3 . . 109.77(5) yes
    O2 P1 O3 . . 110.97(4) yes
    O1 P1 C1 . . 111.26(4) yes
    O2 P1 C1 . . 108.50(4) yes
    O3 P1 C1 . . 100.20(4) yes
    O4 P2 O5 . . 113.28(4) yes
    O4 P2 O6 . . 111.90(5) yes
    O5 P2 O6 . . 111.10(4) yes
    O4 P2 C1 . . 107.38(5) yes
    O5 P2 C1 . . 108.17(4) yes
    O6 P2 C1 . . 104.50(4) yes
    C1 N1 C2 . . 121.58(8) yes
    C1 N1 H2 . . 113.1(10) yes
    C2 N1 H2 . . 112.6(10) yes
    P1 C1 P2 . . 116.39(5) yes
    P1 C1 N1 . . 109.34(6) yes
    P2 C1 N1 . . 110.46(7) yes
    P1 O3 H3 . . 107.4(14) ?
    C2 N2 C6 . . 118.03(9) ?
    N1 C1 H1 . . 107.1(9) ?
    P1 C1 H1 . . 105.3(8) ?
    P2 C1 H1 . . 107.7(8) ?
    N2 C2 N1 . . 118.61(9) ?
    N2 C2 C3 . . 121.53(9) ?
    N1 C2 C3 . . 119.83(9) ?
    C4 C3 C2 . . 118.81(10) ?
    C4 C3 H13 . . 123.3(9) ?
    C2 C3 H13 . . 117.8(9) ?
    C3 C4 C5 . . 120.58(9) ?
    C3 C4 H14 . . 119.5(9) ?
    C5 C4 H14 . . 119.9(9) ?
    C6 C5 C4 . . 115.98(9) ?
    C6 C5 C7 . . 121.31(10) ?
    C4 C5 C7 . . 122.71(9) ?
    N2 C6 C5 . . 125.07(10) ?
    N2 C6 H16 . . 115.2(9) ?
    C5 C6 H16 . . 119.7(9) ?
    C5 C7 H7A . . 111.6(11) ?
    C5 C7 H7B . . 112.9(11) ?
    H7A C7 H7B . . 106.3(14) ?
    C5 C7 H7C . . 112.9(10) ?
    H7A C7 H7C . . 103.8(13) ?
    H7B C7 H7C . . 108.6(14) ?
    H1W O1W H2W . . 103.5(18) ?
    H1N N10 H2N . . 106.2(14) ?
    H1N N10 H3N . . 109.9(16) ?
    H2N N10 H3N . . 108.1(16) ?
    H1N N10 H4N . . 104.8(14) ?
    H2N N10 H4N . . 117.6(15) ?
    H3N N10 H4N . . 110.1(16) ?
    H5N N20 H6N . . 106.2(13) ?
    H5N N20 H7N . . 108.4(14) ?
    H6N N20 H7N . . 111.1(15) ?
    H5N N20 H8N . . 109.1(15) ?
    H6N N20 H8N . . 112.9(15) ?
    H7N N20 H8N . . 108.9(15) ?
    H9N N30 H10N . . 107.4(14) ?
    H9N N30 H11N . . 107.4(15) ?
    H10N N30 H11N . . 111.6(14) ?
    H9N N30 H12N . . 109.3(15) ?
    H10N N30 H12N . . 112.6(15) ?
    H11N N30 H12N . . 108.4(15) ?
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    O1 P1 C1 P2 . . . . 57.76(7) yes
    O2 P1 C1 P2 . . . . -69.88(6) yes
    O3 P1 C1 P2 . . . . 173.79(5) yes
    O4 P2 C1 P1 . . . . -48.06(6) yes
    O5 P2 C1 P1 . . . . 74.53(6) yes
    O6 P2 C1 P1 . . . . -167.04(5) yes
    O1 P1 C1 N1 . . . . -176.25(6) yes
    O2 P1 C1 N1 . . . . 56.11(7) yes
    O3 P1 C1 N1 . . . . -60.22(7) yes
    O4 P2 C1 N1 . . . . -173.48(6) yes
    O5 P2 C1 N1 . . . . -50.90(7) yes
    O6 P2 C1 N1 . . . . 67.53(7) yes
    C2 N1 C1 P1 . . . . 98.98(9) yes
    C2 N1 C1 P2 . . . . -131.69(8) yes
    C1 N1 C2 N2 . . . . 34.58(12) yes
    C1 N1 C2 C3 . . . . -147.18(9) yes
    C6 N2 C2 N1 . . . . 178.27(8) ?
    C6 N2 C2 C3 . . . . 0.07(14) ?
    N2 C2 C3 C4 . . . . -0.53(14) ?
    N1 C2 C3 C4 . . . . -178.71(9) ?
    C2 C3 C4 C5 . . . . 0.80(15) ?
    C3 C4 C5 C6 . . . . -0.60(15) ?
    C3 C4 C5 C7 . . . . 179.42(9) ?
    C2 N2 C6 C5 . . . . 0.14(15) ?
    C4 C5 C6 N2 . . . . 0.12(15) ?
    C7 C5 C6 N2 . . . . -179.90(9) ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    O3 H3 O6 4_565 0.94(2) 1.55(2) 2.4790(10)
                                            174(2)
    O1W H1W O2 . 0.84(2) 1.91(2) 2.742(2) 179(2)
    O1W H2W O3 1_565 0.87(2) 2.07(2) 2.893(2) 157(2)
    N1 H2 O1W . 0.86(2) 2.49(2) 3.315(2) 160(2)
    N10 H1N O5 . 0.90(2) 1.94(2) 2.795(2) 158(2)
    N10 H2N O1 2_655 0.88(2) 2.07(2) 2.927(2) 165(2)
    N10 H3N O1 1_565 0.84(2) 2.20(2) 2.935(2) 145(2)
    N10 H3N O4 1_565 0.84(2) 2.36(2) 2.970(2) 130(2)
    N10 H4N O4 3_666 0.90(2) 1.95(2) 2.845(2) 173(2)
    N20 H5N O1 . 0.89(2) 2.60(2) 3.085(2) 115.0(10)
    N20 H5N O4 . 0.89(2) 1.92(2) 2.774(2) 160(2)
    N20 H6N O5 3_666 0.89(2) 2.05(2) 2.927(2) 172(2)
    N20 H7N O1 2_655 0.88(2) 1.99(2) 2.862(2) 177(2)
    N20 H8N O2 2_645 0.87(2) 1.92(2) 2.760(2) 162(2)
    N30 H9N O6 . 0.88(2) 1.83(2) 2.700(2) 169(2)
    N30 H10N N2 . 0.92(2) 2.03(2) 2.915(2) 160(2)
    N30 H11N O5 1_545 0.90(2) 1.86(2) 2.750(2) 169(2)
    N30 H12N O1W 4_566 0.86(2) 2.13(2) 2.894(2) 149(2)
    C1 H1 N2 . 0.98(2) 2.44(2) 2.892(2) 108.0(10)
