Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S205252061701811X/um5009sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S205252061701811X/um5009Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S205252061701811X/um5009sup3.pdf |
CCDC reference: 1812448
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).
KMn2O10V3 | Z = 2 |
Mr = 461.80 | F(000) = 436 |
Triclinic, P1 | Dx = 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 |
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 | Rint = 0.033 |
ω scans | θmax = 30.0°, θmin = 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 |
Tmin = 0.416, Tmax = 0.853 | k = −9→9 |
8207 measured reflections | l = −13→13 |
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(Fo2) + (0.0253P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.061 | (Δ/σ)max < 0.001 |
S = 1.11 | Δρmax = 0.59 e Å−3 |
2514 reflections | Δρmin = −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) |
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. |
x | y | z | Uiso*/Ueq | ||
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) |
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) |
Mn1—O9i | 2.122 (2) | V2—K1x | 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—O3iv | 2.248 (2) | V3—O2 | 1.8400 (19) |
Mn1—O2 | 2.306 (2) | V3—K1 | 3.7892 (16) |
Mn1—Mn2iv | 3.2202 (15) | V3—K1viii | 3.9280 (17) |
Mn1—K1v | 3.778 (2) | V1—O7 | 1.643 (2) |
Mn1—K1vi | 3.9834 (19) | V1—O9 | 1.6498 (19) |
Mn2—O8 | 2.094 (2) | V1—O5xi | 1.758 (2) |
Mn2—O4vii | 2.138 (2) | V1—O2ii | 1.8364 (18) |
Mn2—O10viii | 2.143 (2) | V1—K1ii | 3.583 (3) |
Mn2—O3 | 2.156 (2) | V1—K1iv | 3.742 (2) |
Mn2—O1 | 2.184 (2) | K1—O8 | 2.610 (2) |
Mn2—O1iv | 2.293 (2) | K1—O6xii | 2.624 (2) |
Mn2—K1 | 3.8347 (16) | K1—O9ii | 2.641 (2) |
Mn2—K1viii | 3.9285 (18) | K1—O7iv | 2.817 (3) |
V2—O8 | 1.672 (2) | K1—O3viii | 3.068 (2) |
V2—O6vii | 1.6817 (18) | K1—O6vi | 3.086 (2) |
V2—O3iv | 1.7227 (18) | K1—O10 | 3.174 (2) |
V2—O5 | 1.8145 (18) | K1—O5 | 3.236 (3) |
V2—K1ix | 3.443 (3) | K1—O10viii | 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) | O5xi—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—K1iv | 44.53 (7) |
O6—Mn1—O7iii | 87.71 (7) | O9—V1—K1iv | 137.74 (7) |
O9i—Mn1—O3iv | 90.11 (6) | O5xi—V1—K1iv | 69.42 (8) |
O4ii—Mn1—O3iv | 83.07 (6) | O2ii—V1—K1iv | 111.94 (6) |
O6—Mn1—O3iv | 175.87 (6) | K1ii—V1—K1iv | 141.35 (4) |
O7iii—Mn1—O3iv | 91.29 (7) | O8—K1—O6xii | 135.70 (7) |
O9i—Mn1—O2 | 92.45 (7) | O8—K1—O9ii | 112.21 (7) |
O4ii—Mn1—O2 | 88.90 (6) | O6xii—K1—O9ii | 109.09 (6) |
O6—Mn1—O2 | 92.56 (6) | O8—K1—O7iv | 71.00 (6) |
O7iii—Mn1—O2 | 171.95 (6) | O6xii—K1—O7iv | 66.40 (6) |
O3iv—Mn1—O2 | 88.98 (6) | O9ii—K1—O7iv | 143.56 (7) |
O9i—Mn1—Mn2iv | 132.02 (6) | O8—K1—O3viii | 147.36 (6) |
O4ii—Mn1—Mn2iv | 41.16 (5) | O6xii—K1—O3viii | 58.06 (7) |
O6—Mn1—Mn2iv | 141.93 (5) | O9ii—K1—O3viii | 77.19 (6) |
O7iii—Mn1—Mn2iv | 86.58 (5) | O7iv—K1—O3viii | 120.76 (6) |
O3iv—Mn1—Mn2iv | 41.91 (5) | O8—K1—O6vi | 104.49 (6) |
O2—Mn1—Mn2iv | 88.26 (4) | O6xii—K1—O6vi | 82.33 (6) |
O9i—Mn1—K1v | 101.83 (5) | O9ii—K1—O6vi | 60.53 (5) |
O4ii—Mn1—K1v | 82.42 (5) | O7iv—K1—O6vi | 83.24 (5) |
O6—Mn1—K1v | 42.32 (6) | O3viii—K1—O6vi | 107.05 (5) |
O7iii—Mn1—K1v | 47.62 (5) | O8—K1—O10 | 87.57 (6) |
O3iv—Mn1—K1v | 137.71 (6) | O6xii—K1—O10 | 109.98 (6) |
O2—Mn1—K1v | 130.09 (5) | O9ii—K1—O10 | 87.17 (7) |
Mn2iv—Mn1—K1v | 113.91 (4) | O7iv—K1—O10 | 129.03 (6) |
O9i—Mn1—K1vi | 37.58 (6) | O3viii—K1—O10 | 61.04 (5) |
O4ii—Mn1—K1vi | 148.34 (5) | O6vi—K1—O10 | 147.69 (6) |
O6—Mn1—K1vi | 50.17 (5) | O8—K1—O5 | 56.35 (6) |
O7iii—Mn1—K1vi | 83.35 (5) | O6xii—K1—O5 | 137.93 (6) |
O3iv—Mn1—K1vi | 125.73 (5) | O9ii—K1—O5 | 63.21 (5) |
O2—Mn1—K1vi | 102.98 (4) | O7iv—K1—O5 | 95.13 (5) |
Mn2iv—Mn1—K1vi | 163.970 (17) | O3viii—K1—O5 | 140.20 (6) |
K1v—Mn1—K1vi | 67.39 (3) | O6vi—K1—O5 | 57.31 (5) |
O8—Mn2—O4vii | 102.27 (6) | O10—K1—O5 | 110.74 (5) |
O8—Mn2—O10viii | 97.48 (7) | O8—K1—O10viii | 63.05 (6) |
O4vii—Mn2—O10viii | 92.26 (7) | O6xii—K1—O10viii | 92.22 (6) |
O8—Mn2—O3 | 164.99 (7) | O9ii—K1—O10viii | 143.25 (5) |
O4vii—Mn2—O3 | 85.38 (6) | O7iv—K1—O10viii | 72.14 (6) |
O10viii—Mn2—O3 | 95.07 (7) | O3viii—K1—O10viii | 90.35 (5) |
O8—Mn2—O1 | 84.99 (7) | O6vi—K1—O10viii | 154.85 (5) |
O4vii—Mn2—O1 | 164.18 (7) | O10—K1—O10viii | 56.98 (7) |
O10viii—Mn2—O1 | 100.79 (7) | O5—K1—O10viii | 118.78 (5) |
O3—Mn2—O1 | 84.61 (6) | O8—K1—V2xiii | 155.14 (5) |
O8—Mn2—O1iv | 82.74 (6) | O6xii—K1—V2xiii | 28.29 (4) |
O4vii—Mn2—O1iv | 84.82 (6) | O9ii—K1—V2xiii | 91.82 (5) |
O10viii—Mn2—O1iv | 177.05 (6) | O7iv—K1—V2xiii | 93.70 (4) |
O3—Mn2—O1iv | 85.15 (6) | O3viii—K1—V2xiii | 29.98 (4) |
O1—Mn2—O1iv | 82.16 (6) | O6vi—K1—V2xiii | 92.57 (4) |
O8—Mn2—Mn1iv | 141.81 (5) | O10—K1—V2xiii | 87.38 (4) |
O4vii—Mn2—Mn1iv | 41.25 (5) | O5—K1—V2xiii | 147.14 (5) |
O10viii—Mn2—Mn1iv | 95.27 (5) | O10viii—K1—V2xiii | 94.05 (4) |
O3—Mn2—Mn1iv | 44.13 (5) | O8—K1—V2 | 26.21 (4) |
O1—Mn2—Mn1iv | 127.50 (5) | O6xii—K1—V2 | 149.12 (5) |
O1iv—Mn2—Mn1iv | 82.83 (4) | O9ii—K1—V2 | 87.88 (5) |
O8—Mn2—K1 | 40.14 (6) | O7iv—K1—V2 | 84.50 (4) |
O4vii—Mn2—K1 | 116.76 (5) | O3viii—K1—V2 | 152.81 (4) |
O10viii—Mn2—K1 | 60.80 (5) | O6vi—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) |
O1iv—Mn2—K1 | 120.22 (5) | O10viii—K1—V2 | 88.25 (4) |
Mn1iv—Mn2—K1 | 149.99 (2) | V2xiii—K1—V2 | 176.51 (3) |
O8—Mn2—K1viii | 133.48 (5) | O8—K1—V1ii | 102.49 (5) |
O4vii—Mn2—K1viii | 113.29 (5) | O6xii—K1—V1ii | 121.77 (4) |
O10viii—Mn2—K1viii | 53.78 (6) | O9ii—K1—V1ii | 25.44 (4) |
O3—Mn2—K1viii | 50.97 (5) | O7iv—K1—V1ii | 164.88 (5) |
O1—Mn2—K1viii | 68.88 (5) | O3viii—K1—V1ii | 72.22 (5) |
O1iv—Mn2—K1viii | 127.92 (5) | O6vi—K1—V1ii | 85.36 (4) |
Mn1iv—Mn2—K1viii | 82.15 (4) | O10—K1—V1ii | 62.62 (4) |
K1—Mn2—K1viii | 95.41 (5) | O5—K1—V1ii | 70.27 (3) |
O8—V2—O6vii | 109.89 (10) | O10viii—K1—V1ii | 117.83 (4) |
O8—V2—O3iv | 112.53 (9) | V2xiii—K1—V1ii | 96.71 (3) |
O6vii—V2—O3iv | 110.04 (9) | V2—K1—V1ii | 84.50 (3) |
O8—V2—O5 | 107.60 (9) | V3—O1—Mn2 | 134.27 (10) |
O6vii—V2—O5 | 112.20 (9) | V3—O1—Mn2iv | 123.39 (10) |
O3iv—V2—O5 | 104.50 (9) | Mn2—O1—Mn2iv | 97.84 (6) |
O8—V2—K1ix | 134.81 (7) | V1ii—O2—V3 | 126.47 (10) |
O6vii—V2—K1ix | 47.68 (6) | V1ii—O2—Mn1 | 117.49 (9) |
O3iv—V2—K1ix | 62.87 (6) | V3—O2—Mn1 | 115.19 (8) |
O5—V2—K1ix | 117.16 (6) | V2iv—O3—Mn2 | 123.88 (10) |
O8—V2—K1 | 43.57 (6) | V2iv—O3—Mn1iv | 129.03 (9) |
O6vii—V2—K1 | 134.77 (7) | Mn2—O3—Mn1iv | 93.95 (6) |
O3iv—V2—K1 | 114.25 (6) | V2iv—O3—K1viii | 87.15 (8) |
O5—V2—K1 | 65.02 (6) | Mn2—O3—K1viii | 95.95 (6) |
K1ix—V2—K1 | 176.51 (3) | Mn1iv—O3—K1viii | 124.85 (7) |
O8—V2—K1x | 128.23 (6) | V3—O4—Mn2xiv | 129.35 (9) |
O6vii—V2—K1x | 48.46 (6) | V3—O4—Mn1ii | 132.58 (10) |
O3iv—V2—K1x | 119.08 (7) | Mn2xiv—O4—Mn1ii | 97.59 (7) |
O5—V2—K1x | 63.86 (7) | V1i—O5—V2 | 130.36 (11) |
K1ix—V2—K1x | 71.15 (3) | V1i—O5—K1 | 134.09 (8) |
K1—V2—K1x | 112.31 (3) | V2—O5—K1 | 84.43 (7) |
O10—V3—O1 | 106.93 (10) | V2xiv—O6—Mn1 | 138.97 (11) |
O10—V3—O4 | 111.79 (9) | V2xiv—O6—K1v | 104.03 (9) |
O1—V3—O4 | 109.89 (9) | Mn1—O6—K1v | 104.24 (7) |
O10—V3—O2 | 108.43 (9) | V2xiv—O6—K1vi | 107.46 (7) |
O1—V3—O2 | 108.69 (8) | Mn1—O6—K1vi | 97.53 (6) |
O4—V3—O2 | 110.97 (9) | K1v—O6—K1vi | 97.67 (6) |
O10—V3—K1 | 56.00 (6) | V1—O7—Mn1iii | 144.61 (11) |
O1—V3—K1 | 84.38 (7) | V1—O7—K1iv | 111.34 (9) |
O4—V3—K1 | 164.35 (6) | Mn1iii—O7—K1iv | 97.89 (6) |
O2—V3—K1 | 68.45 (7) | V2—O8—Mn2 | 129.12 (9) |
O10—V3—K1viii | 58.04 (7) | V2—O8—K1 | 110.22 (9) |
O1—V3—K1viii | 71.28 (7) | Mn2—O8—K1 | 108.71 (8) |
O4—V3—K1viii | 82.99 (8) | V1—O9—Mn1xi | 135.78 (11) |
O2—V3—K1viii | 164.32 (6) | V1—O9—K1ii | 111.13 (10) |
K1—V3—K1viii | 96.15 (5) | Mn1xi—O9—K1ii | 113.08 (8) |
O7—V1—O9 | 107.40 (10) | V3—O10—Mn2viii | 164.34 (11) |
O7—V1—O5xi | 108.65 (10) | V3—O10—K1 | 98.26 (8) |
O9—V1—O5xi | 104.64 (10) | Mn2viii—O10—K1 | 93.22 (6) |
O7—V1—O2ii | 112.46 (9) | V3—O10—K1viii | 97.12 (7) |
O9—V1—O2ii | 108.31 (9) | Mn2viii—O10—K1viii | 85.35 (6) |
O5xi—V1—O2ii | 114.85 (9) | K1—O10—K1viii | 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. |