A novel representative in the rare family of trivanadates, KMn2V3O10: synthesis, crystal structure and magnetic properties

Yakubovich, O.; Shvanskaya, L.; Pchelkina, Z.; Dimitrova, O.; Volkov, A.; Volkova, O.; Vasiliev, A.

doi:10.1107/S205252061701811X

A novel representative in the rare family of trivanadates, KMn₂V₃O₁₀: synthesis, crystal structure and magnetic properties

O. Yakubovich, L. Shvanskaya, Z. Pchelkina, O. Dimitrova, A. Volkov, O. Volkova and A. Vasiliev

Potassium dimanganese trivanadate, KMn₂V₃O₁₀, was synthesized hydrothermally and its crystal structure was determined from single-crystal X-ray diffraction data. The novel phase crystallizes with triclinic symmetry in space group $P\bar 1$ with unit-cell parameters of a = 6.912 (5), b = 6.993 (5), c = 9.656 (5) Å, α = 101.858 (5), β = 102.627 (5), γ = 100.669 (5)°, Z = 2 and V = 432.6 (5) Å³. Its structure is built from tetramers of MnO₆ octahedra sharing edges and trimers of VO₄ tetrahedra sharing vertices. These main structural fragments are linked in a three-dimensional framework with channels occupied by potassium ions. The transformation of this structure to that of interconnected NaCa₃Mn(V₃O₁₀)(V₂O₇) is discussed. The title compound orders antiferromagnetically at T_N = 8.2 K due to the magnetic exchange interactions between tetramers of Mn octahedra through VO₄ tetrahedra. First-principles calculations show the magnetic couplings via Mn—O—Mn and Mn—O—V—O—Mn pathways.

Keywords: crystal structure; trivanadate; anionic framework; magnetic cluster.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S205252061701811X/um5009sup1.cif Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S205252061701811X/um5009Isup2.hkl Contains datablock I
	Portable Document Format (PDF) file https://doi.org/10.1107/S205252061701811X/um5009sup3.pdf Supplementary material

CCDC reference: 1812448

Computing details top

Data collection: CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46); cell refinement: CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46); data reduction: CrysAlis PRO, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46); program(s) used to solve structure: SHELXT (Sheldrick, 2015); program(s) used to refine structure: SHELXL2016/6 (Sheldrick, 2016); molecular graphics: DIMOND (Brandenburg, 2006).

Potassium dimanganese trivanadate top

Crystal data top

KMn₂O₁₀V₃	Z = 2
M_r = 461.80	F(000) = 436
Triclinic, P1	D_x = 3.545 Mg m⁻³
a = 6.912 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 6.993 (5) Å	Cell parameters from 4295 reflections
c = 9.656 (5) Å	θ = 2.7–32.6°
α = 101.858 (5)°	µ = 6.48 mm⁻¹
β = 102.627 (5)°	T = 293 K
γ = 100.669 (5)°	Plate, brown
V = 432.6 (5) Å³	0.42 × 0.10 × 0.05 mm

Data collection top

Xcalibur, Sapphire3 diffractometer	2514 independent reflections
Radiation source: Enhance (Mo) X-ray Source	2293 reflections with I > 2σ(I)
Detector resolution: 16.0630 pixels mm^-1	R_int = 0.033
ω scans	θ_max = 30.0°, θ_min = 3.1°
Absorption correction: gaussian CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Numerical absorption correction based on gaussian integration over a multifaceted crystal model	h = −9→9
T_min = 0.416, T_max = 0.853	k = −9→9
8207 measured reflections	l = −13→13

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.024	w = 1/[σ²(F_o²) + (0.0253P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.061	(Δ/σ)_max < 0.001
S = 1.11	Δρ_max = 0.59 e Å⁻³
2514 reflections	Δρ_min = −0.59 e Å⁻³
146 parameters	Extinction correction: SHELXL-2016/6 (Sheldrick 2016), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0054 (8)

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq
Mn1	−0.05715 (5)	−0.23945 (5)	0.20586 (4)	0.00979 (9)
Mn2	0.68277 (5)	0.20730 (5)	0.51821 (4)	0.00951 (9)
V2	0.45866 (6)	−0.11174 (6)	0.17904 (4)	0.00759 (9)
V3	0.16188 (6)	0.23648 (6)	0.45149 (4)	0.00782 (10)
V1	0.08777 (6)	−0.22435 (6)	0.88229 (4)	0.00812 (10)
K1	0.45437 (9)	0.39821 (10)	0.18908 (8)	0.02634 (16)
O1	0.3568 (2)	0.1315 (3)	0.50399 (18)	0.0112 (3)
O2	0.0248 (3)	0.1073 (3)	0.25920 (18)	0.0113 (3)
O3	0.7223 (2)	0.2313 (3)	0.74941 (18)	0.0107 (3)
O4	0.0021 (3)	0.2181 (3)	0.56376 (18)	0.0116 (3)
O5	0.3122 (3)	−0.0721 (3)	0.01147 (19)	0.0135 (4)
O6	−0.3792 (3)	−0.2570 (3)	0.14679 (19)	0.0129 (3)
O7	0.1326 (3)	−0.4411 (3)	0.8119 (2)	0.0161 (4)
O8	0.5892 (3)	0.1142 (3)	0.28848 (18)	0.0123 (3)
O9	−0.0760 (3)	−0.2680 (3)	0.97995 (19)	0.0166 (4)
O10	0.2639 (3)	0.4749 (3)	0.4604 (2)	0.0171 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mn1	0.00952 (18)	0.01029 (19)	0.00936 (18)	0.00229 (14)	0.00219 (14)	0.00255 (14)
Mn2	0.00880 (17)	0.01070 (18)	0.00832 (17)	0.00199 (14)	0.00138 (14)	0.00215 (14)
V2	0.00708 (18)	0.00747 (19)	0.00774 (19)	0.00174 (14)	0.00131 (15)	0.00162 (15)
V3	0.00743 (19)	0.00801 (19)	0.00777 (19)	0.00202 (14)	0.00170 (15)	0.00169 (15)
V1	0.00799 (18)	0.00896 (19)	0.00753 (18)	0.00234 (15)	0.00125 (15)	0.00296 (15)
K1	0.0154 (3)	0.0207 (3)	0.0455 (4)	0.0034 (2)	0.0040 (3)	0.0194 (3)
O1	0.0094 (8)	0.0114 (8)	0.0131 (8)	0.0040 (7)	0.0024 (7)	0.0032 (7)
O2	0.0125 (8)	0.0102 (8)	0.0104 (8)	0.0029 (7)	0.0013 (7)	0.0027 (7)
O3	0.0090 (8)	0.0124 (8)	0.0112 (8)	0.0015 (7)	0.0034 (7)	0.0044 (7)
O4	0.0108 (8)	0.0145 (9)	0.0093 (8)	0.0034 (7)	0.0029 (7)	0.0018 (7)
O5	0.0112 (8)	0.0154 (9)	0.0124 (8)	−0.0002 (7)	0.0002 (7)	0.0066 (7)
O6	0.0116 (8)	0.0119 (9)	0.0165 (9)	0.0038 (7)	0.0049 (7)	0.0045 (7)
O7	0.0191 (9)	0.0105 (9)	0.0184 (9)	0.0041 (7)	0.0040 (8)	0.0036 (7)
O8	0.0152 (9)	0.0094 (8)	0.0100 (8)	0.0004 (7)	0.0013 (7)	0.0018 (7)
O9	0.0120 (9)	0.0262 (11)	0.0113 (9)	0.0029 (8)	0.0027 (7)	0.0059 (8)
O10	0.0196 (9)	0.0103 (9)	0.0206 (10)	0.0023 (7)	0.0042 (8)	0.0050 (7)

Geometric parameters (Å, º) top

Mn1—O9ⁱ	2.122 (2)	V2—K1^x	3.9323 (18)
Mn1—O4ⁱⁱ	2.142 (2)	V3—O10	1.663 (2)
Mn1—O6	2.147 (2)	V3—O1	1.6830 (18)
Mn1—O7ⁱⁱⁱ	2.160 (2)	V3—O4	1.7144 (18)
Mn1—O3^iv	2.248 (2)	V3—O2	1.8400 (19)
Mn1—O2	2.306 (2)	V3—K1	3.7892 (16)
Mn1—Mn2^iv	3.2202 (15)	V3—K1^viii	3.9280 (17)
Mn1—K1^v	3.778 (2)	V1—O7	1.643 (2)
Mn1—K1^vi	3.9834 (19)	V1—O9	1.6498 (19)
Mn2—O8	2.094 (2)	V1—O5^xi	1.758 (2)
Mn2—O4^vii	2.138 (2)	V1—O2ⁱⁱ	1.8364 (18)
Mn2—O10^viii	2.143 (2)	V1—K1ⁱⁱ	3.583 (3)
Mn2—O3	2.156 (2)	V1—K1^iv	3.742 (2)
Mn2—O1	2.184 (2)	K1—O8	2.610 (2)
Mn2—O1^iv	2.293 (2)	K1—O6^xii	2.624 (2)
Mn2—K1	3.8347 (16)	K1—O9ⁱⁱ	2.641 (2)
Mn2—K1^viii	3.9285 (18)	K1—O7^iv	2.817 (3)
V2—O8	1.672 (2)	K1—O3^viii	3.068 (2)
V2—O6^vii	1.6817 (18)	K1—O6^vi	3.086 (2)
V2—O3^iv	1.7227 (18)	K1—O10	3.174 (2)
V2—O5	1.8145 (18)	K1—O5	3.236 (3)
V2—K1^ix	3.443 (3)	K1—O10^viii	3.359 (2)
V2—K1	3.553 (3)

O9ⁱ—Mn1—O4ⁱⁱ	173.03 (6)	O7—V1—K1ⁱⁱ	97.08 (8)
O9ⁱ—Mn1—O6	86.00 (7)	O9—V1—K1ⁱⁱ	43.43 (7)
O4ⁱⁱ—Mn1—O6	100.78 (6)	O5^xi—V1—K1ⁱⁱ	145.00 (6)
O9ⁱ—Mn1—O7ⁱⁱⁱ	95.60 (7)	O2ⁱⁱ—V1—K1ⁱⁱ	74.18 (6)
O4ⁱⁱ—Mn1—O7ⁱⁱⁱ	83.15 (7)	O7—V1—K1^iv	44.53 (7)
O6—Mn1—O7ⁱⁱⁱ	87.71 (7)	O9—V1—K1^iv	137.74 (7)
O9ⁱ—Mn1—O3^iv	90.11 (6)	O5^xi—V1—K1^iv	69.42 (8)
O4ⁱⁱ—Mn1—O3^iv	83.07 (6)	O2ⁱⁱ—V1—K1^iv	111.94 (6)
O6—Mn1—O3^iv	175.87 (6)	K1ⁱⁱ—V1—K1^iv	141.35 (4)
O7ⁱⁱⁱ—Mn1—O3^iv	91.29 (7)	O8—K1—O6^xii	135.70 (7)
O9ⁱ—Mn1—O2	92.45 (7)	O8—K1—O9ⁱⁱ	112.21 (7)
O4ⁱⁱ—Mn1—O2	88.90 (6)	O6^xii—K1—O9ⁱⁱ	109.09 (6)
O6—Mn1—O2	92.56 (6)	O8—K1—O7^iv	71.00 (6)
O7ⁱⁱⁱ—Mn1—O2	171.95 (6)	O6^xii—K1—O7^iv	66.40 (6)
O3^iv—Mn1—O2	88.98 (6)	O9ⁱⁱ—K1—O7^iv	143.56 (7)
O9ⁱ—Mn1—Mn2^iv	132.02 (6)	O8—K1—O3^viii	147.36 (6)
O4ⁱⁱ—Mn1—Mn2^iv	41.16 (5)	O6^xii—K1—O3^viii	58.06 (7)
O6—Mn1—Mn2^iv	141.93 (5)	O9ⁱⁱ—K1—O3^viii	77.19 (6)
O7ⁱⁱⁱ—Mn1—Mn2^iv	86.58 (5)	O7^iv—K1—O3^viii	120.76 (6)
O3^iv—Mn1—Mn2^iv	41.91 (5)	O8—K1—O6^vi	104.49 (6)
O2—Mn1—Mn2^iv	88.26 (4)	O6^xii—K1—O6^vi	82.33 (6)
O9ⁱ—Mn1—K1^v	101.83 (5)	O9ⁱⁱ—K1—O6^vi	60.53 (5)
O4ⁱⁱ—Mn1—K1^v	82.42 (5)	O7^iv—K1—O6^vi	83.24 (5)
O6—Mn1—K1^v	42.32 (6)	O3^viii—K1—O6^vi	107.05 (5)
O7ⁱⁱⁱ—Mn1—K1^v	47.62 (5)	O8—K1—O10	87.57 (6)
O3^iv—Mn1—K1^v	137.71 (6)	O6^xii—K1—O10	109.98 (6)
O2—Mn1—K1^v	130.09 (5)	O9ⁱⁱ—K1—O10	87.17 (7)
Mn2^iv—Mn1—K1^v	113.91 (4)	O7^iv—K1—O10	129.03 (6)
O9ⁱ—Mn1—K1^vi	37.58 (6)	O3^viii—K1—O10	61.04 (5)
O4ⁱⁱ—Mn1—K1^vi	148.34 (5)	O6^vi—K1—O10	147.69 (6)
O6—Mn1—K1^vi	50.17 (5)	O8—K1—O5	56.35 (6)
O7ⁱⁱⁱ—Mn1—K1^vi	83.35 (5)	O6^xii—K1—O5	137.93 (6)
O3^iv—Mn1—K1^vi	125.73 (5)	O9ⁱⁱ—K1—O5	63.21 (5)
O2—Mn1—K1^vi	102.98 (4)	O7^iv—K1—O5	95.13 (5)
Mn2^iv—Mn1—K1^vi	163.970 (17)	O3^viii—K1—O5	140.20 (6)
K1^v—Mn1—K1^vi	67.39 (3)	O6^vi—K1—O5	57.31 (5)
O8—Mn2—O4^vii	102.27 (6)	O10—K1—O5	110.74 (5)
O8—Mn2—O10^viii	97.48 (7)	O8—K1—O10^viii	63.05 (6)
O4^vii—Mn2—O10^viii	92.26 (7)	O6^xii—K1—O10^viii	92.22 (6)
O8—Mn2—O3	164.99 (7)	O9ⁱⁱ—K1—O10^viii	143.25 (5)
O4^vii—Mn2—O3	85.38 (6)	O7^iv—K1—O10^viii	72.14 (6)
O10^viii—Mn2—O3	95.07 (7)	O3^viii—K1—O10^viii	90.35 (5)
O8—Mn2—O1	84.99 (7)	O6^vi—K1—O10^viii	154.85 (5)
O4^vii—Mn2—O1	164.18 (7)	O10—K1—O10^viii	56.98 (7)
O10^viii—Mn2—O1	100.79 (7)	O5—K1—O10^viii	118.78 (5)
O3—Mn2—O1	84.61 (6)	O8—K1—V2^xiii	155.14 (5)
O8—Mn2—O1^iv	82.74 (6)	O6^xii—K1—V2^xiii	28.29 (4)
O4^vii—Mn2—O1^iv	84.82 (6)	O9ⁱⁱ—K1—V2^xiii	91.82 (5)
O10^viii—Mn2—O1^iv	177.05 (6)	O7^iv—K1—V2^xiii	93.70 (4)
O3—Mn2—O1^iv	85.15 (6)	O3^viii—K1—V2^xiii	29.98 (4)
O1—Mn2—O1^iv	82.16 (6)	O6^vi—K1—V2^xiii	92.57 (4)
O8—Mn2—Mn1^iv	141.81 (5)	O10—K1—V2^xiii	87.38 (4)
O4^vii—Mn2—Mn1^iv	41.25 (5)	O5—K1—V2^xiii	147.14 (5)
O10^viii—Mn2—Mn1^iv	95.27 (5)	O10^viii—K1—V2^xiii	94.05 (4)
O3—Mn2—Mn1^iv	44.13 (5)	O8—K1—V2	26.21 (4)
O1—Mn2—Mn1^iv	127.50 (5)	O6^xii—K1—V2	149.12 (5)
O1^iv—Mn2—Mn1^iv	82.83 (4)	O9ⁱⁱ—K1—V2	87.88 (5)
O8—Mn2—K1	40.14 (6)	O7^iv—K1—V2	84.50 (4)
O4^vii—Mn2—K1	116.76 (5)	O3^viii—K1—V2	152.81 (4)
O10^viii—Mn2—K1	60.80 (5)	O6^vi—K1—V2	84.26 (4)
O3—Mn2—K1	146.11 (5)	O10—K1—V2	96.07 (4)
O1—Mn2—K1	77.83 (5)	O5—K1—V2	30.55 (4)
O1^iv—Mn2—K1	120.22 (5)	O10^viii—K1—V2	88.25 (4)
Mn1^iv—Mn2—K1	149.99 (2)	V2^xiii—K1—V2	176.51 (3)
O8—Mn2—K1^viii	133.48 (5)	O8—K1—V1ⁱⁱ	102.49 (5)
O4^vii—Mn2—K1^viii	113.29 (5)	O6^xii—K1—V1ⁱⁱ	121.77 (4)
O10^viii—Mn2—K1^viii	53.78 (6)	O9ⁱⁱ—K1—V1ⁱⁱ	25.44 (4)
O3—Mn2—K1^viii	50.97 (5)	O7^iv—K1—V1ⁱⁱ	164.88 (5)
O1—Mn2—K1^viii	68.88 (5)	O3^viii—K1—V1ⁱⁱ	72.22 (5)
O1^iv—Mn2—K1^viii	127.92 (5)	O6^vi—K1—V1ⁱⁱ	85.36 (4)
Mn1^iv—Mn2—K1^viii	82.15 (4)	O10—K1—V1ⁱⁱ	62.62 (4)
K1—Mn2—K1^viii	95.41 (5)	O5—K1—V1ⁱⁱ	70.27 (3)
O8—V2—O6^vii	109.89 (10)	O10^viii—K1—V1ⁱⁱ	117.83 (4)
O8—V2—O3^iv	112.53 (9)	V2^xiii—K1—V1ⁱⁱ	96.71 (3)
O6^vii—V2—O3^iv	110.04 (9)	V2—K1—V1ⁱⁱ	84.50 (3)
O8—V2—O5	107.60 (9)	V3—O1—Mn2	134.27 (10)
O6^vii—V2—O5	112.20 (9)	V3—O1—Mn2^iv	123.39 (10)
O3^iv—V2—O5	104.50 (9)	Mn2—O1—Mn2^iv	97.84 (6)
O8—V2—K1^ix	134.81 (7)	V1ⁱⁱ—O2—V3	126.47 (10)
O6^vii—V2—K1^ix	47.68 (6)	V1ⁱⁱ—O2—Mn1	117.49 (9)
O3^iv—V2—K1^ix	62.87 (6)	V3—O2—Mn1	115.19 (8)
O5—V2—K1^ix	117.16 (6)	V2^iv—O3—Mn2	123.88 (10)
O8—V2—K1	43.57 (6)	V2^iv—O3—Mn1^iv	129.03 (9)
O6^vii—V2—K1	134.77 (7)	Mn2—O3—Mn1^iv	93.95 (6)
O3^iv—V2—K1	114.25 (6)	V2^iv—O3—K1^viii	87.15 (8)
O5—V2—K1	65.02 (6)	Mn2—O3—K1^viii	95.95 (6)
K1^ix—V2—K1	176.51 (3)	Mn1^iv—O3—K1^viii	124.85 (7)
O8—V2—K1^x	128.23 (6)	V3—O4—Mn2^xiv	129.35 (9)
O6^vii—V2—K1^x	48.46 (6)	V3—O4—Mn1ⁱⁱ	132.58 (10)
O3^iv—V2—K1^x	119.08 (7)	Mn2^xiv—O4—Mn1ⁱⁱ	97.59 (7)
O5—V2—K1^x	63.86 (7)	V1ⁱ—O5—V2	130.36 (11)
K1^ix—V2—K1^x	71.15 (3)	V1ⁱ—O5—K1	134.09 (8)
K1—V2—K1^x	112.31 (3)	V2—O5—K1	84.43 (7)
O10—V3—O1	106.93 (10)	V2^xiv—O6—Mn1	138.97 (11)
O10—V3—O4	111.79 (9)	V2^xiv—O6—K1^v	104.03 (9)
O1—V3—O4	109.89 (9)	Mn1—O6—K1^v	104.24 (7)
O10—V3—O2	108.43 (9)	V2^xiv—O6—K1^vi	107.46 (7)
O1—V3—O2	108.69 (8)	Mn1—O6—K1^vi	97.53 (6)
O4—V3—O2	110.97 (9)	K1^v—O6—K1^vi	97.67 (6)
O10—V3—K1	56.00 (6)	V1—O7—Mn1ⁱⁱⁱ	144.61 (11)
O1—V3—K1	84.38 (7)	V1—O7—K1^iv	111.34 (9)
O4—V3—K1	164.35 (6)	Mn1ⁱⁱⁱ—O7—K1^iv	97.89 (6)
O2—V3—K1	68.45 (7)	V2—O8—Mn2	129.12 (9)
O10—V3—K1^viii	58.04 (7)	V2—O8—K1	110.22 (9)
O1—V3—K1^viii	71.28 (7)	Mn2—O8—K1	108.71 (8)
O4—V3—K1^viii	82.99 (8)	V1—O9—Mn1^xi	135.78 (11)
O2—V3—K1^viii	164.32 (6)	V1—O9—K1ⁱⁱ	111.13 (10)
K1—V3—K1^viii	96.15 (5)	Mn1^xi—O9—K1ⁱⁱ	113.08 (8)
O7—V1—O9	107.40 (10)	V3—O10—Mn2^viii	164.34 (11)
O7—V1—O5^xi	108.65 (10)	V3—O10—K1	98.26 (8)
O9—V1—O5^xi	104.64 (10)	Mn2^viii—O10—K1	93.22 (6)
O7—V1—O2ⁱⁱ	112.46 (9)	V3—O10—K1^viii	97.12 (7)
O9—V1—O2ⁱⁱ	108.31 (9)	Mn2^viii—O10—K1^viii	85.35 (6)
O5^xi—V1—O2ⁱⁱ	114.85 (9)	K1—O10—K1^viii	123.02 (7)

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

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