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The crystal structure of barium tetra­ammonium poly{hexa­kis[phosphate(V)]} was solved by direct methods from laboratory X-ray powder diffraction data collected at room temperature. The trigonal crystal structure is isostructural with BaCs4(PO3)6. The Ba2+ cation and one of the N atoms lie on a threefold axis, whereas all remaining non-H atoms are in general positions. The Ba2+ cation is bonded to nine O atoms from three polyphosphate chains to form a distorted tricapped trigonal prism as coordination polyhedron. Links between the polyphosphate chains and the Ba2+ ions result in a three-dimensional network, with tunnels and cavities filled by ammonium cations.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806053864/wm2082sup1.cif
Contains datablocks global, I

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S1600536806053864/wm2082Isup2.rtv
Contains datablock I

Key indicators

  • Powder X-ray study
  • T = 295 K
  • Mean [sigma](P-O) = 0.016 Å
  • R factor = 0.000
  • wR factor = 0.000
  • Data-to-parameter ratio = 0.0

checkCIF/PLATON results

No syntax errors found



Alert level C REFI023_ALERT_1_C _refine_diff_density_max is missing Maximum value of final difference map (e A-3). The following tests will not be performed DIFMN_01,DIFMX_01,DIFMX_02 REFI024_ALERT_1_C _refine_diff_density_min is missing Minimum value of final difference map (e A-3). The following tests will not be performed DIFMN_01,DIFMN_02,DIFMN_03
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: local program; cell refinement: FULLPROF (Rodrigues-Carvajal, 2001); data reduction: local program; program(s) used to solve structure: EXPO (Altomare et al., 1999); program(s) used to refine structure: FULLPROF; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: FULLPROF and PLATON (Spek, 2003).

Babarium tetraammonium poly{hexakis[phosphate(V)]} top
Crystal data top
Ba(NH4)4(PO3)6F(000) = 668.0
Mr = 683.32Dx = 2.340 Mg m3
Trigonal, P31cCu Kα radiation, λ = 1.5418 Å
Hall symbol: P 3 -2cT = 295 K
a = 11.1936 (2) ÅParticle morphology: needle-like
c = 8.9393 (3) Åcolourless
V = 970.00 (4) Å3flat_sheet, 30 × 30 mm
Z = 2Specimen preparation: Prepared at 295 K
Data collection top
Carl Zeiss (Jena) HZG-4A
diffractometer
Data collection mode: reflection
Radiation source: fine-focus sealed X-ray tube, BSV-29Scan method: step
Ni filtered monochromator2θmin = 8°, 2θmax = 105°, 2θstep = 0.02°
Specimen mounting: packed powder pellet
Refinement top
Refinement on Inet49 parameters
Least-squares matrix: full with fixed elements per cycle10 restraints
Rp = 0.066H-atom parameters constrained
Rwp = 0.089Weighting scheme based on measured s.u.'s
Rexp = 0.156(Δ/σ)max = 0.001
RBragg = 0.045Background function: polynomial, with six refined coefficients
4851 data pointsPreferred orientation correction: Marsh–Dollase function (Marsh, 1932; Dollase, 1986); correction for the [001] preferred orientation of needle-like grains; refined parameters G1 = 1.39(2), G2 = 0.09(4).
Profile function: pseudo-Voight; the refined value of the η parameter is 0.692(13).
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba0.666670.333330.250000.0126 (18)*
P10.4440 (8)0.4557 (8)0.4793 (7)0.0090 (11)*
P20.2948 (6)0.2758 (5)0.2286 (6)0.0090 (11)*
O10.441 (4)0.574 (3)0.535 (5)0.014 (2)*
O20.583 (2)0.459 (3)0.482 (5)0.014 (2)*
O30.3681 (17)0.4137 (13)0.3229 (16)0.014 (2)*
O40.1441 (14)0.2042 (16)0.265 (5)0.014 (2)*
O50.3715 (12)0.2049 (15)0.274 (4)0.014 (2)*
O60.3159 (18)0.322 (2)0.0563 (14)0.014 (2)*
N10.666660.333330.730640.014 (2)*
H10.666670.333330.635640.05000*
H20.603100.348000.762280.05000*
N20.008 (6)0.232 (3)0.518 (7)0.014 (2)*
H30.039290.205100.446450.05000*
H40.070960.309810.547500.05000*
H50.061490.236920.487870.05000*
H60.018050.173540.589210.05000*
Geometric parameters (Å, º) top
Ba—O1i2.73 (5)P2—O31.581 (14)
Ba—O1ii2.73 (5)P2—O41.50 (2)
Ba—O1iii2.73 (5)P2—O51.488 (19)
Ba—O22.91 (2)P2—O61.604 (14)
Ba—O2iv2.91 (2)N1—H10.8500
Ba—O2v2.91 (2)N1—H20.8500
Ba—O52.877 (17)N1—H2iv0.8500
Ba—O5iv2.877 (17)N1—H2v0.8500
Ba—O5v2.877 (17)N2—H30.8500
P1—O11.43 (4)N2—H40.8400
P1—O21.54 (3)N2—H50.8500
P1—O31.581 (17)N2—H60.8500
P1—O6vi1.628 (19)
O1—P1—O2118 (2)P1i—O6—P2127.0 (12)
O1—P1—O3109 (2)H1—N1—H2109.00
O1—P1—O6vi110.2 (19)H1—N1—H2iv109.00
O2—P1—O3114.1 (18)H1—N1—H2v109.00
O2—P1—O6vi111.6 (16)H2—N1—H2iv110.00
O3—P1—O6vi91.2 (9)H2—N1—H2v110.00
O3—P2—O4107.6 (14)H2iv—N1—H2v110.00
O3—P2—O5102.7 (12)H3—N2—H4109.00
O3—P2—O6106.0 (9)H3—N2—H5110.00
O4—P2—O5116.8 (12)H3—N2—H6109.00
O4—P2—O6109.0 (18)H4—N2—H5111.00
O5—P2—O6113.8 (16)H4—N2—H6110.00
P1—O3—P2134.5 (11)H5—N2—H6108.00
O1—P1—O3—P2157 (2)O4—P2—O3—P194 (2)
O2—P1—O3—P269 (2)O5—P2—O3—P130 (2)
O6vi—P1—O3—P245 (2)O6—P2—O3—P1149.3 (18)
O1—P1—O6vi—P2vi42 (3)O3—P2—O6—P1i42 (2)
O2—P1—O6vi—P2vi91 (2)O4—P2—O6—P1i157.5 (16)
O3—P1—O6vi—P2vi152.3 (18)O5—P2—O6—P1i70.2 (18)
Symmetry codes: (i) y, x, z1/2; (ii) xy+1, y+1, z1/2; (iii) x+1, x+y, z1/2; (iv) y+1, xy, z; (v) x+y+1, x+1, z; (vi) y, x, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O20.852.46003.02 (4)124.0
N1—H1···O2iv0.852.46003.02 (4)124.0
N1—H1···O2v0.852.46003.02 (4)124.0
N1—H2···O3vi0.852.31003.155 (17)172.0
N2—H3···O40.852.00002.83 (7)162.0
N2—H4···O1vii0.842.52003.20 (5)139.0
N2—H4···O5vi0.842.41003.02 (7)130.0
N2—H5···O5viii0.852.36003.04 (7)136.0
N2—H5···O2vii0.852.44003.10 (7)135.0
N2—H6···O4ix0.852.07002.86 (7)155.0
Symmetry codes: (iv) y+1, xy, z; (v) x+y+1, x+1, z; (vi) y, x, z+1/2; (vii) x+y, x+1, z; (viii) y, xy, z; (ix) x, x+y, z+1/2.
 

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