Tetrakis(3,5-xylidinium) dihydrogen cyclohexaphosphate dihydrate
Marouani, Houda; Rzaigui, Mohamed; Acta Crystallographica Section E 66 (2010) o233–; doi:10.1107/S1600536809054452

data_2224648
_publ_section_title
;
 Tetrakis(3,5-xylidinium) dihydrogen cyclohexaphosphate dihydrate
;
_journal_coeditor_code           HB5267
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o233
_journal_paper_doi               10.1107/S1600536809054452
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '4C8 H12 N +, H2 P6 O18 4-, 2H2 O'
_chemical_formula_moiety         '4(C8 H12 N +), H2 O18 P6 4-, 2(H2 O)'
_chemical_formula_sum            'C32 H54 N4 O20 P6'
_chemical_formula_weight         1000.61
_chemical_name_systematic
;
Tetrakis(3,5-xylidinium) dihydrogen 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                 106.41(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.254(3)
_cell_length_b                   11.763(5)
_cell_length_c                   11.556(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.1
_cell_measurement_theta_min      6.3
_cell_volume                     2249.9(12)
_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)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10097
_diffrn_reflns_theta_full        34.96
_diffrn_reflns_theta_max         34.96
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        11
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.512
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         9844
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0664P)^2^+0.0078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                5567
_reflns_number_total             9844
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5267.cif
_cod_data_source_block           I
_cod_original_cell_volume        2249.9(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2224648
_cod_database_fobs_code          2224648