Bis(3-azoniapentane-1,5-diaminium) cyclohexaphosphate dihydrate: a monoclinic polymorph
Khedhiri, Lamia; Akriche, Samah; Al-Deyab, Salem S.; Rzaigui, Mohamed; Acta Crystallographica Section E 68 (2012) o2038–o2039; doi:10.1107/S1600536812025172

data_2235450
_publ_section_title
;
 Bis(3-azoniapentane-1,5-diaminium) cyclohexaphosphate dihydrate: a
 monoclinic polymorph
;
_journal_coeditor_code           HB6809
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2038
_journal_page_last               o2039
_journal_paper_doi               10.1107/S1600536812025172
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '2C4 H16 N3 3+, P6 O18 6-, 2H2 O'
_chemical_formula_moiety         ' 2(C4 H16 N3 3+), P6 O18 6-, 2(H2 O)'
_chemical_formula_sum            'C8 H36 N6 O20 P6'
_chemical_formula_weight         722.25
_chemical_name_systematic
;
Bis(3-azoniapentane-1,5-diaminium) cyclohexaphosphate dihydrate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.07(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.033(4)
_cell_length_b                   16.597(2)
_cell_length_c                   8.007(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9
_cell_volume                     1287.5(7)
_computing_cell_refinement       'CAD-4 Express (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 Express (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
;
Ortep-3 (Farrugia, 1997) and DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9091
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.967
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         6303
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+0.1509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                5211
_reflns_number_total             6303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            hb6809.cif
_cod_data_source_block           I
_cod_original_cell_volume        1287.6(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2235450
_cod_database_fobs_code          2235450