#------------------------------------------------------------------------------
#$Date: 2025-08-19 21:17:10 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301807 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/11/2241193.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241193
loop_
_publ_author_name
'Leinemann, Malte'
'Jess, Inke'
'Boeckmann, Jan'
'Näther, Christian'
_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 et al., 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/[σ²(Fo²)+(0.0636P)²+0.3897P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2.014
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
O O1 0.6408(2) 0.5792(2) 0.5089(3) 0.0230(5) Uani d 1
H H1O1 0.6827 0.5567 0.4562 0.035 Uiso calc 1
N N1 0.5202(3) 0.4522(2) 0.5550(2) 0.0203(5) Uani d 1
H H1N1 0.5515 0.4032 0.6016 0.030 Uiso calc 1
H H2N1 0.4668 0.3955 0.4922 0.030 Uiso calc 1
H H3N1 0.4649 0.4767 0.6008 0.030 Uiso calc 1
P P1 0.3333 0.6667 0.64509(11) 0.0166(3) Uani d 1
O O2 0.3333 0.6667 0.5059(3) 0.0223(8) Uani d 1
O O3 0.3977(2) 0.5747(2) 0.69256(18) 0.0202(5) Uani d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 O1 H1O1 . . 109.5
O1 N1 H1N1 . . 109.5
O1 N1 H2N1 . . 109.5
H1N1 N1 H2N1 . . 109.5
O1 N1 H3N1 . . 109.5
H1N1 N1 H3N1 . . 109.5
H2N1 N1 H3N1 . . 109.5
O2 P1 O3 . 2_665 109.77(9)
O2 P1 O3 . 3_565 109.77(9)
O3 P1 O3 2_665 3_565 109.17(9)
O2 P1 O3 . . 109.77(9)
O3 P1 O3 2_665 . 109.17(9)
O3 P1 O3 3_565 . 109.17(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 N1 . 1.421(3) y
O1 H1O1 . 0.8400 ?
N1 H1N1 . 0.9100 ?
N1 H2N1 . 0.9100 ?
N1 H3N1 . 0.9100 ?
P1 O2 . 1.535(4) y
P1 O3 2_665 1.548(2) ?
P1 O3 3_565 1.548(2) ?
P1 O3 . 1.548(2) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1O1 O3 14_654 0.84 1.70 2.540(3) 172.3
N1 H1N1 O2 16_654 0.91 1.90 2.785(3) 163.3
N1 H2N1 O1 12_454 0.91 2.37 3.110(4) 137.9
N1 H2N1 O3 15_554 0.91 2.20 2.884(3) 131.5
N1 H3N1 O3 . 0.91 1.84 2.732(3) 164.4
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 10176537
