Crystal structure of tris(hydroxylammonium) orthophosphate
Leinemann, Malte; Jess, Inke; Boeckmann, Jan; Näther, Christian; Acta Crystallographica Section E 71 (2015) i10–i11; doi:10.1107/S2056989015018642

data_2241193
_publ_section_title
;
 Crystal structure of tris(hydroxylammonium) orthophosphate
;
_journal_coeditor_code           WM5223
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i10
_journal_page_last               i11
_journal_paper_doi               10.1107/S2056989015018642
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '3H4 N O +, P O4 3-'
_chemical_formula_moiety         '3(H4 N O +), P O4 3-'
_chemical_formula_sum            'H12 N3 O7 P'
_chemical_formula_weight         197.10
_chemical_name_systematic
;
Tris(hydroxylammonium) orthophosphate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   10.7072(9)
_cell_length_b                   10.7072(9)
_cell_length_c                   11.0283(13)
_cell_measurement_reflns_used    5420
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      59.17
_cell_measurement_theta_min      7.64
_cell_volume                     1094.94(18)
_computing_cell_refinement       'X-Area (Stoe, 2008)'
_computing_data_collection       'X-Area (Stoe, 2008)'
_computing_data_reduction        'X-Area (Stoe, 2008)'
_computing_molecular_graphics
'XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'publcif (Westrip, 2010)'
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5420
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.980
_diffrn_reflns_theta_min         3.806
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.324
_refine_ls_abs_structure_details
;
 Flack x determined using 287 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons <i>et al</i>., 2013)
;
_refine_ls_abs_structure_Flack   -0.06(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         647
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.3897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                621
_reflns_number_total             647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5223sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1094.9(2)
_cod_database_code               2241193
_cod_database_fobs_code          2241193
_shelx_hkl_checksum              91916
_shelx_res_checksum              71914
_shelxl_version_number           2.014