Crystal structure of barium dinickel(II) iron(III) tris­[orthophosphate(V)], BaNi₂Fe(PO₄)₃

The orthophosphate BaNi₂Fe(PO₄)₃ crystallizes in the α-CrPO₄ type of structure, in which edge-sharing [Ni₂O₁₀] octa­hedra are linked to PO₄ tetra­hedra and [FeO₆] octa­hedra to form a three-dimensional framework delimiting channels which house disordered Ba²⁺ cations.

Key indicators

Structure: I

• Single-crystal X-ray study
• T = 296 K
• Mean [sigma](P-O) = 0.001 Å
• Disorder in main residue
• R factor = 0.015
• wR factor = 0.036
• Data-to-parameter ratio = 25.2

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT975_ALERT_2_C Check Calcd Resid. Dens.  0.94Ang From O3      .       0.46 eA-3

Alert level G
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          2 Info
PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...      0.250 Check
PLAT300_ALERT_4_G Atom Site Occupancy of Ba2        Constrained at     0.0132 Check
PLAT300_ALERT_4_G Atom Site Occupancy of Ba1        Constrained at     0.9868 Check
PLAT301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )         0% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  2  )       100% Note
PLAT794_ALERT_5_G Tentative Bond Valency for Ni1       (II)      .       1.89 Info
PLAT933_ALERT_2_G Number of HKL-OMIT Records in Embedded .res File          1 Note
PLAT965_ALERT_2_G The SHELXL WEIGHT Optimisation has not Converged     Please Check

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   2 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   9 ALERT level G = General information/check it is not something unexpected

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

---

Computing details

Data collection: APEX3 (Bruker, 2016); cell refinement: SAINT (Bruker, 2016); data reduction: SAINT (Bruker, 2016); program(s) used to solve structure: SHELXT2014/4 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015b); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012), DIAMOND (Brandenburg, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

Barium dinickel(II) iron(III) tris[orthophosphate(V)]

Crystal data

BaNi2Fe(PO4)3	Dx = 4.327 Mg m^−3
Mr = 595.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Imma	Cell parameters from 1460 reflections
a = 10.4711 (2) Å	θ = 3.1–39.4°
b = 13.2007 (3) Å	µ = 10.46 mm^−1
c = 6.6132 (1) Å	T = 296 K
V = 914.12 (3) Å^3	Block, colourless
Z = 4	0.32 × 0.25 × 0.19 mm
F(000) = 1116

Data collection

Bruker X8 APEX Diffractometer	1460 independent reflections
Radiation source: fine-focus sealed tube	1440 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.029
φ and ω scans	θmax = 39.4°, θmin = 3.1°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −18→13
Tmin = 0.624, Tmax = 0.748	k = −23→23
18099 measured reflections	l = −11→11

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.015	w = 1/[σ^2(Fo^2) + (0.0147P)^2 + 1.8221P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.036	(Δ/σ)max = 0.001
S = 1.21	Δρmax = 1.33 e Å^−3
1460 reflections	Δρmin = −0.78 e Å^−3
58 parameters	Extinction correction: SHELXL2018/3 (Sheldrick, 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00403 (16)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ba1	0.500000	0.250000	0.39902 (2)	0.00770 (4)	0.9868
Ba2	1.000000	0.500000	1.000000	0.020 (2)	0.0132
Ni1	0.750000	0.36701 (2)	0.750000	0.00501 (4)
Fe1	1.000000	0.500000	0.500000	0.00337 (5)
P1	0.500000	0.250000	0.90454 (8)	0.00317 (8)
P2	0.750000	0.57020 (3)	0.750000	0.00365 (6)
O1	0.500000	0.34524 (8)	1.03493 (17)	0.00581 (16)
O2	0.61939 (10)	0.250000	0.76536 (17)	0.00534 (15)
O3	0.78276 (8)	0.63385 (6)	0.93423 (13)	0.00771 (12)
O4	0.86254 (7)	0.49395 (6)	0.70839 (12)	0.00574 (11)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ba1	0.00681 (5)	0.01253 (6)	0.00377 (5)	0.000	0.000	0.000
Ba2	0.014 (5)	0.041 (8)	0.006 (4)	0.000	0.000	0.000 (4)
Ni1	0.00498 (7)	0.00383 (7)	0.00621 (8)	0.000	0.00057 (5)	0.000
Fe1	0.00303 (10)	0.00352 (10)	0.00355 (10)	0.000	0.000	0.00008 (8)
P1	0.00348 (18)	0.00281 (17)	0.00322 (18)	0.000	0.000	0.000
P2	0.00380 (13)	0.00392 (13)	0.00324 (12)	0.000	0.00055 (10)	0.000
O1	0.0078 (4)	0.0033 (3)	0.0063 (4)	0.000	0.000	−0.0014 (3)
O2	0.0042 (4)	0.0063 (4)	0.0055 (4)	0.000	0.0016 (3)	0.000
O3	0.0096 (3)	0.0080 (3)	0.0055 (3)	−0.0024 (2)	0.0007 (2)	−0.0023 (2)
O4	0.0045 (3)	0.0058 (3)	0.0070 (3)	0.0009 (2)	0.0016 (2)	0.0006 (2)

Geometric parameters (Å, º)

Ba1—O1^i	2.7163 (11)	Ni1—O4	2.0670 (8)
Ba1—O1^ii	2.7163 (11)	Ni1—O4^xii	2.0670 (8)
Ba1—O2^iii	2.7262 (11)	Ni1—O3^x	2.1163 (8)
Ba1—O2	2.7262 (11)	Ni1—O3^iv	2.1163 (8)
Ba1—O3^iv	2.7530 (8)	Fe1—O4	1.9944 (8)
Ba1—O3^v	2.7530 (8)	Fe1—O4^ix	1.9944 (8)
Ba1—O3^vi	2.7530 (8)	Fe1—O4^xiii	1.9944 (8)
Ba1—O3^vii	2.7530 (8)	Fe1—O4^xiv	1.9944 (8)
Ba2—O4	2.4077 (8)	Fe1—O1^iv	2.0559 (11)
Ba2—O4^viii	2.4078 (8)	Fe1—O1^xv	2.0559 (11)
Ba2—O4^ix	2.4078 (8)	P1—O1	1.5246 (11)
Ba2—O4^x	2.4078 (8)	P1—O1^iii	1.5246 (11)
Ba2—O3^ix	2.9129 (9)	P1—O2	1.5524 (11)
Ba2—O3^x	2.9129 (9)	P1—O2^iii	1.5524 (11)
Ba2—O3^viii	2.9129 (9)	P2—O3	1.5192 (8)
Ba2—O3	2.9129 (9)	P2—O3^xii	1.5193 (8)
Ni1—O2^xi	2.0655 (7)	P2—O4^xii	1.5739 (8)
Ni1—O2	2.0655 (7)	P2—O4	1.5739 (8)
O1^i—Ba1—O1^ii	55.14 (4)	O4^viii—Ba2—O3	124.49 (2)
O1^i—Ba1—O2^iii	141.97 (2)	O4^ix—Ba2—O3	111.55 (2)
O1^ii—Ba1—O2^iii	141.97 (2)	O4^x—Ba2—O3	68.45 (2)
O1^i—Ba1—O2	141.97 (2)	O3^ix—Ba2—O3	102.68 (3)
O1^ii—Ba1—O2	141.97 (2)	O3^x—Ba2—O3	77.32 (3)
O2^iii—Ba1—O2	54.59 (5)	O3^viii—Ba2—O3	180.0
O1^i—Ba1—O3^iv	109.44 (2)	O2^xi—Ni1—O2	83.20 (5)
O1^ii—Ba1—O3^iv	79.47 (2)	O2^xi—Ni1—O4	102.84 (3)
O2^iii—Ba1—O3^iv	107.68 (3)	O2—Ni1—O4	172.00 (3)
O2—Ba1—O3^iv	63.00 (2)	O2^xi—Ni1—O4^xii	172.00 (4)
O1^i—Ba1—O3^v	79.47 (2)	O2—Ni1—O4^xii	102.84 (3)
O1^ii—Ba1—O3^v	109.44 (2)	O4—Ni1—O4^xii	71.66 (4)
O2^iii—Ba1—O3^v	63.00 (2)	O2^xi—Ni1—O3^x	86.40 (4)
O2—Ba1—O3^v	107.68 (3)	O2—Ni1—O3^x	93.14 (4)
O3^iv—Ba1—O3^v	170.30 (4)	O4—Ni1—O3^x	92.48 (3)
O1^i—Ba1—O3^vi	79.47 (2)	O4^xii—Ni1—O3^x	88.02 (3)
O1^ii—Ba1—O3^vi	109.44 (2)	O2^xi—Ni1—O3^iv	93.14 (4)
O2^iii—Ba1—O3^vi	107.68 (3)	O2—Ni1—O3^iv	86.40 (4)
O2—Ba1—O3^vi	63.00 (2)	O4—Ni1—O3^iv	88.02 (3)
O3^iv—Ba1—O3^vi	67.69 (4)	O4^xii—Ni1—O3^iv	92.48 (3)
O3^v—Ba1—O3^vi	111.43 (4)	O3^x—Ni1—O3^iv	179.39 (5)
O1^i—Ba1—O3^vii	109.44 (2)	O2^xi—Ni1—P2	138.40 (2)
O1^ii—Ba1—O3^vii	79.47 (2)	O2—Ni1—P2	138.40 (2)
O2^iii—Ba1—O3^vii	63.00 (2)	O4—Fe1—O4^ix	92.40 (5)
O2—Ba1—O3^vii	107.68 (3)	O4—Fe1—O4^xiii	87.60 (5)
O3^iv—Ba1—O3^vii	111.43 (4)	O4^ix—Fe1—O4^xiii	180.0
O3^v—Ba1—O3^vii	67.69 (4)	O4—Fe1—O4^xiv	180.0
O3^vi—Ba1—O3^vii	170.30 (4)	O4^ix—Fe1—O4^xiv	87.60 (5)
O4—Ba2—O4^viii	180.0	O4^xiii—Fe1—O4^xiv	92.40 (5)
O4—Ba2—O4^ix	73.43 (4)	O4—Fe1—O1^iv	87.83 (3)
O4^viii—Ba2—O4^ix	106.57 (4)	O4^ix—Fe1—O1^iv	87.83 (3)
O4—Ba2—O4^x	106.57 (4)	O4^xiii—Fe1—O1^iv	92.17 (3)
O4^viii—Ba2—O4^x	73.43 (4)	O4^xiv—Fe1—O1^iv	92.17 (3)
O4^ix—Ba2—O4^x	180.0	O4—Fe1—O1^xv	92.17 (3)
O4—Ba2—O3^ix	111.55 (2)	O4^ix—Fe1—O1^xv	92.17 (3)
O4^viii—Ba2—O3^ix	68.45 (2)	O4^xiii—Fe1—O1^xv	87.83 (3)
O4^ix—Ba2—O3^ix	55.51 (2)	O4^xiv—Fe1—O1^xv	87.83 (3)
O4^x—Ba2—O3^ix	124.49 (2)	O1^iv—Fe1—O1^xv	180.0
O4—Ba2—O3^x	68.45 (2)	O1—P1—O1^iii	111.11 (9)
O4^viii—Ba2—O3^x	111.55 (2)	O1—P1—O2	109.59 (3)
O4^ix—Ba2—O3^x	124.49 (2)	O1^iii—P1—O2	109.59 (3)
O4^x—Ba2—O3^x	55.51 (2)	O1—P1—O2^iii	109.59 (3)
O3^ix—Ba2—O3^x	180.0	O1^iii—P1—O2^iii	109.59 (3)
O4—Ba2—O3^viii	124.49 (2)	O2—P1—O2^iii	107.28 (9)
O4^viii—Ba2—O3^viii	55.51 (2)	O3—P2—O3^xii	112.84 (7)
O4^ix—Ba2—O3^viii	68.45 (2)	O3—P2—O4^xii	112.49 (4)
O4^x—Ba2—O3^viii	111.55 (2)	O3^xii—P2—O4^xii	108.95 (5)
O3^ix—Ba2—O3^viii	77.32 (3)	O3—P2—O4	108.95 (5)
O3^x—Ba2—O3^viii	102.68 (3)	O3^xii—P2—O4	112.49 (4)
O4—Ba2—O3	55.51 (2)	O4^xii—P2—O4	100.50 (6)

Symmetry codes: (i) −x+1, −y+1/2, z−1; (ii) x, y, z−1; (iii) −x+1, −y+1/2, z; (iv) −x+3/2, −y+1, z−1/2; (v) x−1/2, y−1/2, z−1/2; (vi) −x+3/2, y−1/2, z−1/2; (vii) x−1/2, −y+1, z−1/2; (viii) −x+2, −y+1, −z+2; (ix) −x+2, y, z; (x) x, −y+1, −z+2; (xi) −x+3/2, −y+1/2, −z+3/2; (xii) −x+3/2, y, −z+3/2; (xiii) x, −y+1, −z+1; (xiv) −x+2, −y+1, −z+1; (xv) x+1/2, y, −z+3/2.