Tris(methylammonium) hydrogenphosphate dihydrogenphosphate
Fábry, Jan; Krupková, Radmila; Vaněk, Přemysl; Dušek, Michal; Acta Crystallographica Section C 62 (2006) o73–o75; doi:10.1107/S0108270105041934

data_2014345
_publ_section_title
;
 Tris(methylammonium) hydrogenphosphate dihydrogenphosphate
;
_journal_coeditor_code           GG1289
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o73
_journal_page_last               o75
_journal_paper_doi               10.1107/S0108270105041934
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '3C H6 N + , H O4 P 2- , H2 O4 P -'
_chemical_formula_moiety         '3C H6 N + , H O4 P 2- , H2 O4 P -'
_chemical_formula_sum            'C3 H21 N3 O8 P2'
_chemical_formula_weight         289.2
_chemical_name_systematic
;
Tris(methylammonium) hydrogenphosphate dihydrogenphosphate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_cell_angle_alpha                90
_cell_angle_beta                 95.556(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3571(6)
_cell_length_b                   6.5465(2)
_cell_length_c                   15.1231(6)
_cell_measurement_reflns_used    20259
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      3.31
_cell_volume                     1217.65(9)
_computing_cell_refinement       'Crysalis RED (Oxford Diffraction, 2005)'
_computing_data_collection       'Crysalis CCD (Oxford Diffraction, 2005)'
_computing_data_reduction        'Crysalis RED'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2003)'
_computing_publication_material  JANA2000
_computing_structure_refinement  'JANA2000 (Pet\<r\'i\<cek & Du\<sek, 2000)'
_computing_structure_solution    'SIR97 (Altomare et al.,  1999)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Model CCD area-detector'
_diffrn_measurement_method
;
Rotation method data acquisition using \w scans
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0097
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20259
_diffrn_reflns_reduction_process
;
Integration of the CCD images was done by program Crysalis RED
The same program was used for indexing of the
crystal shape, its refinement and absorption correction.
;
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         3.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.39
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[Crysalis RED (Oxford Diffraction, 2005); method by Clark & Reid
(1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.5768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.89
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    69
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2498
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.032
_refine_ls_R_factor_gt           0.026
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(I)+0.0009I^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.080
_reflns_number_gt                2187
_reflns_number_total             2498
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            gg1289.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2014345
_cod_database_fobs_code          2014345