Irreversible Phase Transition of Bistetramethylammonium Hydrogencyclotriphosphate
Mangstl, Martin; Celinski, Vinicius R.; Pritzel, Christian; Trettin, Reinhard; Schmedt auf der Günne, Jörn; Zeitschrift für anorganische und allgemeine Chemie 643 (2017) 1609–1614; doi:10.1002/zaac.201700246

data_1570299
_publ_section_title
;
 Irreversible Phase Transition of Bistetramethylammonium
 Hydrogencyclotriphosphate
;
_journal_issue                   21
_journal_name_full
'Zeitschrift f\"ur anorganische und allgemeine Chemie'
_journal_page_first              1609
_journal_page_last               1614
_journal_paper_doi               10.1002/zaac.201700246
_journal_volume                  643
_journal_year                    2017
_chemical_formula_moiety         '2(C4 H12 N), (H P3 O9)'
_chemical_formula_sum            'C8 H25 N2 O9 P3'
_chemical_formula_weight         386.21
_chemical_name_common
'Bistetramethylammonium hydrogencyclo-triphosphate'
_chemical_name_systematic
'Bistetramethylammonium hydrogencyclo-triphosphate'
_chemical_properties_physical
'air-sensitive, moisture-sensitive, hygroscopic'
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           'TOPAS ACADEMIC 4.1 + PLATON'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.382790(86)
_cell_length_b                   11.81960(9)
_cell_length_c                   16.03958(15)
_cell_measurement_temperature    294
_cell_measurement_theta_max      73.99
_cell_measurement_theta_min      4.00
_cell_volume                     1778.80(3)
_computing_molecular_graphics    'Diamond 3.0'
_computing_publication_material  'TOPAS ACADEMIC 4.1'
_computing_structure_refinement  'TOPAS ACADEMIC 4.1'
_computing_structure_solution    'FOX 2016.2'
_diffrn_ambient_pressure         1000
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device_type  'STOE Stadi P'
_diffrn_radiation_monochromator  Ge-111
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.540596
_diffrn_reflns_number            555
_diffrn_reflns_theta_max         73.99
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'STOE sealed Cu tube'
_exptl_absorpt_coefficient_mu    3.476
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.4421
_exptl_crystal_description       microcrystalline
_exptl_crystal_F_000             822.07
_exptl_crystal_recrystallization_method 'from DMSO/CH3CN '
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  colourless
_pd_char_particle_morphology     powder
_pd_meas_number_of_points        7000
_pd_proc_ls_prof_R_factor        0.02183
_pd_proc_ls_prof_wR_factor       0.02905
_pd_proc_number_of_points        7000
_refine_ls_goodness_of_fit_all   1.610
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     121
_refine_ls_number_restraints     20
_refine_ls_R_Fsqd_factor         0.01471
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.00
_reflns_d_resolution_high        9.515
_reflns_d_resolution_low         1.275
_reflns_limit_h_max              7
_reflns_limit_h_min              0
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_total             555
_cod_data_source_file            beta-bisTMA_hydrogencyclotriphosphate.cif
_cod_data_source_block           phase_1
_cod_original_cell_volume        1778.803(28)
_cod_database_code               1570299
_pd_proc_ls_prof_r_expected      0.01804