Hexakis(melaminium) tetrakis(dihydrogenphosphate) monohydrogenphosphate tetrahydrate
Janczak, Jan; Perpétuo, Genivaldo Julio; Acta Crystallographica Section C 58 (2002) o455–o459; doi:10.1107/S0108270102010521

data_2012873
_publ_section_title
;
 Hexakis(melaminium) tetrakis(dihydrogenphosphate)
 monohydrogenphosphate tetrahydrate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o455
_journal_page_last               o459
_journal_paper_doi               10.1107/S0108270102010521
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         '6C3 H7 N6 + , 4H2 O4 P - , H O4 P 2- , 4H2 O'
_chemical_formula_sum            'C18 H59 N36 O24 P5'
_chemical_formula_weight         1318.86
_chemical_melting_point          dehydrated
_chemical_name_common            'melaminium phosphate hydrate'
_chemical_name_systematic
;
hexakis(2,4,6-triamino-1,3,5-triazin-1-ium) tetrakis(dihydrogenphosphate)
monohydrogenphosphate tetrahydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 117.80(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.341(2)
_cell_length_b                   20.965(4)
_cell_length_c                   12.334(2)
_cell_measurement_reflns_used    4999
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2.7
_cell_volume                     2594.1(11)
_computing_cell_refinement       'KM-4 CCD Software'
_computing_data_collection       'KM-4 CCD Software (Kuma Diffraction, 2000)'
_computing_data_reduction        'KM-4 CCD Software'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type
'Kuma KM-4 with two dimensional CCD area-detector'
_diffrn_measurement_method       '\w scan'
_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  0.014
_diffrn_reflns_av_sigmaI/netI    0.026
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25398
_diffrn_reflns_theta_full        29.06
_diffrn_reflns_theta_max         29.06
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'face-indexed (SHELXTL; Sheldrick, 1990)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_meas      1.69
_exptl_crystal_density_method    flotation
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.28
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.11(4)
_refine_ls_extinction_coef       0.00059(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         12689
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.030
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0333P)^2^+0.2410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.062
_refine_ls_wR_factor_ref         0.067
_reflns_number_gt                10664
_reflns_number_total             12689
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd1207.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2012873
_cod_database_fobs_code          2012873