Conformational isomers of the [(5-methyl-2-pyridinio)aminomethylene]diphosphonate dianion and [(5-methyl-2-pyridyl)aminomethylene]diphosphonate trianion in salts with 4-aminopyridine and ammonia
Matczak-Jon, Ewa; Ślepokura, Katarzyna; Kafarski, Paweł; Skrzyńska, Izabela; Jon, Marek; Acta Crystallographica Section C 65 (2009) o261–o266; doi:10.1107/S0108270109010683

data_2017160
_publ_section_title
;
 Conformational isomers of the
 [(5-methyl-2-pyridinio)aminomethylene]diphosphonate dianion and
 [(5-methyl-2-pyridyl)aminomethylene]diphosphonate trianion in salts
 with 4-aminopyridine and ammonia
;
_journal_coeditor_code           TR3053
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o261
_journal_page_last               o266
_journal_paper_doi               10.1107/S0108270109010683
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '3N H4 +, C7 H9 N2 O6 P2 3-, H2 O'
_chemical_formula_moiety         '3(N H4 +), C7 H9 N2 O6 P2 3-, H2 O'
_chemical_formula_sum            'C7 H23 N5 O7 P2'
_chemical_formula_weight         351.24
_chemical_name_systematic
;
triammonium hydrogen [(5-methyl-2-pyridyl)aminomethylene]diphosphonate
monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 109.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.087(3)
_cell_length_b                   6.216(2)
_cell_length_c                   15.159(3)
_cell_measurement_reflns_used    14567
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.74
_cell_measurement_theta_min      2.85
_cell_volume                     1514.5(7)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics
'XP in SHELXTL (Version 5.1; Sheldrick, 2008) and DIAMOND (Brandenburg, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type
'KUMA KM-4 CCD \k-geometry diffractometer with Sapphire CCD camera'
_diffrn_measurement_method       \w
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21075
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         36.83
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         6808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+0.1044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                5206
_reflns_number_total             6808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            tr3053.cif
_cod_data_source_block           II
_cod_original_cell_volume        1514.5(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017160
_cod_database_fobs_code          2017160