Conformations and resulting hydrogen-bonded networks of hydrogen {phosphono[(pyridin-1-ium-3-yl)amino]methyl}phosphonate and related 2-chloro and 6-chloro derivatives
Matczak-Jon, Ewa; Ślepokura, Katarzyna; Acta Crystallographica Section C 67 (2011) o450–o456; doi:10.1107/S0108270111040650

data_2018275
_publ_section_title
;
 Conformations and resulting hydrogen-bonded networks of hydrogen
 {phosphono[(pyridin-1-ium-3-yl)amino]methyl}phosphonate and related
 2-chloro and 6-chloro derivatives
;
_journal_coeditor_code           FG3227
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o450
_journal_page_last               o456
_journal_paper_doi               10.1107/S0108270111040650
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C6 H10 N2 O6 P2 , H2 O'
_chemical_formula_moiety         'C6 H10 N2 O6 P2, H2 O'
_chemical_formula_sum            'C6 H12 N2 O7 P2'
_chemical_formula_weight         286.12
_chemical_name_systematic
;
hydrogen {phosphono[(pyridin-1-ium-3-yl)amino]methyl}phosphonate
monohydrate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 103.55(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.068(3)
_cell_length_b                   7.513(2)
_cell_length_c                   16.126(4)
_cell_measurement_reflns_used    4599
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      36.59
_cell_measurement_theta_min      3.00
_cell_volume                     1068.1(5)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics
;
XP (Bruker, 1998) and DIAMOND (Brandenburg, 2005)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.929
_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         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9984
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2907
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0497P)^2^+1.2174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                2229
_reflns_number_total             2907
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3227.cif
_cod_data_source_block           Ia
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2018275
_cod_database_fobs_code          2018275