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_2017159
_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          '2C5 H7 N2 +, C7 H10 N2 O6 P2 2-, 2.4H2 O'
_chemical_formula_moiety
'2(C5 H7 N2 +), C7 H10 N2 O6 P2 2-, 2.4(H2 O)'
_chemical_formula_sum            'C17 H28.8 N6 O8.4 P2'
_chemical_formula_weight         513.60
_chemical_name_systematic
;
bis(4-aminopyridinium) hydrogen
[(5-methyl-2-pyridinio)aminomethylene]diphosphonate 2.4-hydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.89(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.385(3)
_cell_length_b                   17.838(3)
_cell_length_c                   13.038(3)
_cell_measurement_reflns_used    27791
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.85
_cell_measurement_theta_min      2.78
_cell_volume                     4639.3(16)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38561
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6761
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0589P)^2^+4.7126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                5813
_reflns_number_total             6761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            tr3053.cif
_cod_data_source_block           I
_cod_original_cell_volume        4639.3(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C17 H28.80 N6 O8.40 P2'
_cod_database_code               2017159
_cod_database_fobs_code          2017159