4,4'-Methylenedianilinium hemi(cyclotetraphosphate)
Nahouane, Rachid; Soumhi, El Hassane; Saadoune, Ismael; Driss, Ahmed; Acta Crystallographica Section E 61 (2005) o2850–o2852; doi:10.1107/S1600536805025043

data_2206792
_publ_section_title
;
 4,4'-Methylenedianilinium hemi(cyclotetraphosphate)
;
_journal_coeditor_code           SJ6128
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2850
_journal_page_last               o2852
_journal_paper_doi               10.1107/S1600536805025043
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '2C13 H16 N2 2+, P4 O12 4-'
_chemical_formula_moiety         '2(C13 H16 N2 2+), O12 P4 4-'
_chemical_formula_sum            'C26 H32 N4 O12 P4'
_chemical_formula_weight         716.44
_chemical_name_common            'C26 H32 N4 P4 O12'
_chemical_name_systematic
;
Bis(4,4'-diphenylmethylendiammonium) cyclotetraphosphate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.62(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.467(2)
_cell_length_b                   13.808(3)
_cell_length_c                   14.453(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1619.1(6)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection
'CAD-4 EXPRESS (Duisenberg, 1992; Mac\'i\<cek & Yordanov, 1992)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics
;
ATOMS for Windows (Dowty, 1995) and ORTEPII (Johnson, 1976)
;
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_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  0.0130
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4086
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.47
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.261
_refine_ls_extinction_coef       0.007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0384
_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^)+(0.1136P)^2^+1.5906P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1176
_reflns_number_gt                2874
_reflns_number_total             3528
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj6128.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2019-10-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1619.2(6)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_original_formula_moiety     'C13 H16 N2 2+, 0.5O12 P4 4-'
_cod_original_formula_iupac      'C13 H16 N2 2+, 0.5P4 O12 4-'
_cod_original_formula_sum        'C13 H16 N2 O6 P2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     358.22
_cod_database_code               2206792
_cod_database_fobs_code          2206792