Bis(3-ammoniomethylpyridinium) cyclotetraphosphate
Hemissi, Hanène; Rzaigui, Mohammed; Al-Deyab, Salem S.; Acta Crystallographica Section E 66 (2010) o779–o780; doi:10.1107/S1600536810008056

data_2225504
_publ_section_title
;
 Bis(3-ammoniomethylpyridinium) cyclotetraphosphate
;
_journal_coeditor_code           DN2541
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o779
_journal_page_last               o780
_journal_paper_doi               10.1107/S1600536810008056
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '2C6 H10 N2 2+ , P4 O12 4-'
_chemical_formula_moiety         '2(C6 H10 N2 2+), O12 P4 4-'
_chemical_formula_sum            'C12 H20 N4 O12 P4'
_chemical_formula_weight         536.20
_chemical_name_systematic
;
Bis(3-ammoniomethylpyridinium) cyclotetraphosphate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.24(2)
_cell_angle_beta                 98.73(3)
_cell_angle_gamma                108.76(3)
_cell_formula_units_Z            1
_cell_length_a                   7.849(2)
_cell_length_b                   8.384(2)
_cell_length_c                   9.448(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.65
_cell_measurement_theta_min      9.02
_cell_volume                     512.4(3)
_computing_cell_refinement       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1996)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.0121
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -6
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_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.471
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         5005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0490P)^2^+0.1514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                3963
_reflns_number_total             5005
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2541.cif
_cod_data_source_block           I
_cod_original_cell_volume        512.4(2)
_cod_database_code               2225504
_cod_database_fobs_code          2225504