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Triniobium decaselenide trichloride, Nb3Se10Cl3, contains waved one-dimensional chains in which the Nb atoms are arranged in a sequence of two consecutive short bonds and one long distance. Two Nb atoms are each coordinated by three Se22−, Cl− and μ2-Cl−, whereas the third Nb atom is surrounded by four Se22− to form distorted rectangular antiprisms of Se. Weak interchain interactions between Se and terminal Cl atoms connect the chains along the [101] direction to form a pseudo-two-dimensional layer. Nb3Se10Cl3 is an insulator, in accordance with the charge-balanced formulation [Nb5+][Nb4+]2[Se22−]5[Cl−]3.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (Se-Se) = 0.002 Å
- R factor = 0.055
- wR factor = 0.141
- Data-to-parameter ratio = 24.7
checkCIF/PLATON results
No syntax errors found
Alert level C
DIFMX01_ALERT_2_C The maximum difference density is > 0.1*ZMAX*0.75
_refine_diff_density_max given = 3.507
Test value = 3.075
DIFMX02_ALERT_1_C The maximum difference density is > 0.1*ZMAX*0.75
The relevant atom site should be identified.
PLAT097_ALERT_2_C Maximum (Positive) Residual Density ............ 3.51 e/A
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 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
Data collection: RAPID-AUTO (Rigaku, 2005); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: locally modified version of ORTEP (Johnson, 1965); software used to prepare material for publication: WinGX (Farrugia, 1999).
Triniobium decaselenide trichloride
top
Crystal data top
Nb3Se10Cl3 | F(000) = 2056 |
Mr = 1174.68 | Dx = 4.844 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yb | Cell parameters from 10764 reflections |
a = 7.207 (3) Å | θ = 3.0–27.5° |
b = 18.974 (8) Å | µ = 25.17 mm−1 |
c = 11.834 (7) Å | T = 150 K |
β = 95.60 (2)° | Needle, black |
V = 1610.6 (14) Å3 | 0.30 × 0.10 × 0.05 mm |
Z = 4 | |
Data collection top
Rigaku R-AXIS Rapid diffractometer | 2794 reflections with I > 2σ(I) |
ω scans | Rint = 0.080 |
Absorption correction: numerical (NUMABS; Higashi, 2000) | θmax = 27.5°, θmin = 3.0° |
Tmin = 0.053, Tmax = 0.278 | h = −9→9 |
15892 measured reflections | k = −23→24 |
3799 independent reflections | l = −15→15 |
Refinement top
Refinement on F2 | 154 parameters |
Least-squares matrix: full | 0 restraints |
R[F2 > 2σ(F2)] = 0.055 | w = 1/[σ2(Fo2) + (0.0624P)2 + 20.4571P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.141 | (Δ/σ)max < 0.001 |
S = 1.07 | Δρmax = 3.51 e Å−3 |
3799 reflections | Δρmin = −2.66 e Å−3 |
Special details top
Geometry. All e.s.d.'s are estimated using the full covariance matrix. The cell e.s.d.'s
are taken into account individually in the estimation of e.s.d.'s in
distances, angles and torsion angles; correlations between e.s.d.'s in cell
parameters are only used when they are defined by crystal symmetry. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Nb1 | 0.14692 (15) | 0.14950 (5) | 0.15458 (9) | 0.0163 (2) | |
Nb2 | 0.24186 (15) | 0.00022 (5) | 0.25164 (9) | 0.0166 (2) | |
Nb3 | 0.33033 (15) | 0.64911 (5) | 0.34990 (9) | 0.0164 (2) | |
Se1 | 0.02939 (17) | 0.61199 (7) | 0.21969 (11) | 0.0215 (3) | |
Se2 | 0.06429 (18) | 0.56996 (7) | 0.40624 (11) | 0.0227 (3) | |
Se3 | −0.07300 (18) | 0.42588 (7) | 0.26403 (12) | 0.0226 (3) | |
Se4 | 0.19677 (18) | 0.11482 (7) | 0.36995 (11) | 0.0217 (3) | |
Se5 | 0.21090 (19) | 0.03467 (7) | 0.03457 (11) | 0.0240 (3) | |
Se6 | 0.55234 (18) | 0.53713 (7) | 0.37425 (12) | 0.0255 (3) | |
Se7 | 0.46162 (18) | 0.08523 (7) | 0.14088 (12) | 0.0249 (3) | |
Se8 | 0.50649 (19) | 0.58792 (7) | 0.19658 (12) | 0.0245 (3) | |
Se9 | 0.2741 (3) | 0.25 | 0.01955 (16) | 0.0231 (4) | |
Se10 | 0.5968 (2) | 0.75 | 0.34996 (17) | 0.0236 (4) | |
Se11 | 0.4065 (2) | 0.25 | 0.20525 (16) | 0.0221 (4) | |
Se12 | 0.3732 (3) | 0.75 | 0.19538 (16) | 0.0223 (4) | |
Cl1 | 0.4090 (5) | 0.65224 (18) | 0.5597 (3) | 0.0282 (7) | |
Cl2 | −0.1323 (4) | 0.34744 (17) | 0.0121 (3) | 0.0275 (7) | |
Cl3 | 0.1212 (6) | 0.75 | 0.4059 (4) | 0.0215 (9) | |
Cl4 | −0.0371 (6) | 0.25 | 0.2331 (4) | 0.0231 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nb1 | 0.0214 (5) | 0.0136 (5) | 0.0135 (5) | 0.0002 (4) | 0.0000 (4) | 0.0010 (4) |
Nb2 | 0.0208 (5) | 0.0151 (5) | 0.0138 (5) | 0.0008 (5) | 0.0013 (4) | 0.0012 (4) |
Nb3 | 0.0210 (5) | 0.0137 (5) | 0.0144 (5) | 0.0005 (4) | 0.0005 (4) | −0.0007 (4) |
Se1 | 0.0217 (6) | 0.0214 (6) | 0.0206 (7) | 0.0016 (5) | −0.0013 (5) | −0.0018 (5) |
Se2 | 0.0280 (6) | 0.0214 (6) | 0.0196 (7) | −0.0028 (5) | 0.0064 (5) | −0.0045 (5) |
Se3 | 0.0230 (6) | 0.0213 (6) | 0.0238 (7) | −0.0007 (5) | 0.0047 (5) | −0.0038 (5) |
Se4 | 0.0284 (6) | 0.0211 (6) | 0.0154 (6) | 0.0005 (5) | 0.0017 (5) | 0.0002 (5) |
Se5 | 0.0309 (7) | 0.0241 (6) | 0.0166 (7) | 0.0018 (6) | 0.0015 (5) | −0.0008 (5) |
Se6 | 0.0252 (6) | 0.0238 (7) | 0.0263 (7) | 0.0034 (6) | −0.0034 (5) | −0.0038 (5) |
Se7 | 0.0250 (6) | 0.0202 (6) | 0.0302 (8) | −0.0002 (5) | 0.0061 (5) | 0.0041 (6) |
Se8 | 0.0297 (7) | 0.0204 (6) | 0.0249 (7) | −0.0039 (6) | 0.0098 (5) | −0.0034 (5) |
Se9 | 0.0324 (9) | 0.0209 (9) | 0.0168 (9) | 0 | 0.0058 (7) | 0 |
Se10 | 0.0214 (8) | 0.0208 (9) | 0.0284 (10) | 0 | 0.0004 (8) | 0 |
Se11 | 0.0230 (9) | 0.0206 (9) | 0.0222 (10) | 0 | −0.0010 (7) | 0 |
Se12 | 0.0285 (9) | 0.0217 (9) | 0.0168 (9) | 0 | 0.0030 (7) | 0 |
Cl1 | 0.0351 (17) | 0.0310 (17) | 0.0176 (16) | 0.0026 (15) | −0.0019 (13) | −0.0001 (13) |
Cl2 | 0.0289 (15) | 0.0292 (16) | 0.0231 (17) | 0.0013 (14) | −0.0053 (13) | 0.0014 (14) |
Cl3 | 0.0210 (19) | 0.0175 (19) | 0.026 (2) | 0 | 0.0046 (17) | 0 |
Cl4 | 0.033 (2) | 0.0147 (19) | 0.022 (2) | 0 | 0.0052 (18) | 0 |
Geometric parameters (Å, º) top
Nb1—Cl2i | 2.497 (3) | Nb3—Cl1 | 2.492 (4) |
Nb1—Cl4 | 2.549 (3) | Nb3—Cl3 | 2.563 (3) |
Nb1—Se3i | 2.5761 (19) | Nb3—Se2 | 2.5741 (18) |
Nb1—Se7 | 2.5942 (19) | Nb3—Se8 | 2.589 (2) |
Nb1—Se4 | 2.623 (2) | Nb3—Se1 | 2.6311 (19) |
Nb1—Se5 | 2.6654 (19) | Nb3—Se6 | 2.6586 (19) |
Nb1—Se11 | 2.6975 (18) | Nb3—Se12 | 2.686 (2) |
Nb1—Se9 | 2.7047 (19) | Nb3—Se10 | 2.7114 (19) |
Nb2—Se4 | 2.6234 (19) | Nb1—Nb2 | 3.1075 (18) |
Nb2—Se1i | 2.6283 (18) | Nb2—Nb3i | 3.1053 (19) |
Nb2—Se5 | 2.639 (2) | Se1—Se2 | 2.338 (2) |
Nb2—Se6i | 2.6423 (19) | Se3—Se4i | 2.339 (2) |
Nb2—Se8i | 2.6649 (18) | Se5—Se7 | 2.308 (2) |
Nb2—Se3i | 2.6837 (19) | Se6—Se8 | 2.307 (2) |
Nb2—Se2i | 2.6861 (19) | Se9—Se11 | 2.309 (3) |
Nb2—Se7 | 2.6895 (19) | Se10—Se12 | 2.317 (3) |
| | | |
Cl2i—Nb1—Cl4 | 79.34 (13) | Se8i—Nb2—Nb1 | 128.22 (6) |
Cl2i—Nb1—Se3i | 81.81 (10) | Se3i—Nb2—Nb1 | 52.20 (4) |
Cl4—Nb1—Se3i | 82.23 (9) | Se2i—Nb2—Nb1 | 126.96 (5) |
Cl2i—Nb1—Se7 | 128.37 (10) | Se7—Nb2—Nb1 | 52.57 (4) |
Cl4—Nb1—Se7 | 149.71 (11) | Nb3i—Nb2—Nb1 | 179.08 (5) |
Se3i—Nb1—Se7 | 110.80 (6) | Cl1—Nb3—Cl3 | 78.87 (13) |
Cl2i—Nb1—Se4 | 133.39 (10) | Cl1—Nb3—Se2 | 81.88 (9) |
Cl4—Nb1—Se4 | 81.98 (11) | Cl3—Nb3—Se2 | 84.09 (9) |
Se3i—Nb1—Se4 | 53.47 (5) | Cl1—Nb3—Se8 | 128.99 (10) |
Se7—Nb1—Se4 | 84.55 (6) | Cl3—Nb3—Se8 | 149.00 (11) |
Cl2i—Nb1—Se5 | 80.16 (9) | Se2—Nb3—Se8 | 110.40 (6) |
Cl4—Nb1—Se5 | 158.25 (11) | Cl1—Nb3—Se1 | 133.16 (10) |
Se3i—Nb1—Se5 | 87.76 (6) | Cl3—Nb3—Se1 | 83.07 (10) |
Se7—Nb1—Se5 | 52.03 (5) | Se2—Nb3—Se1 | 53.36 (5) |
Se4—Nb1—Se5 | 107.35 (6) | Se8—Nb3—Se1 | 84.38 (6) |
Cl2i—Nb1—Se11 | 129.01 (9) | Cl1—Nb3—Se6 | 80.51 (9) |
Cl4—Nb1—Se11 | 76.37 (10) | Cl3—Nb3—Se6 | 158.70 (12) |
Se3i—Nb1—Se11 | 136.73 (7) | Se2—Nb3—Se6 | 87.78 (6) |
Se7—Nb1—Se11 | 75.79 (6) | Se8—Nb3—Se6 | 52.15 (5) |
Se4—Nb1—Se11 | 86.28 (6) | Se1—Nb3—Se6 | 107.61 (6) |
Se5—Nb1—Se11 | 122.96 (7) | Cl1—Nb3—Se12 | 129.12 (10) |
Cl2i—Nb1—Se9 | 83.22 (10) | Cl3—Nb3—Se12 | 75.73 (10) |
Cl4—Nb1—Se9 | 84.61 (10) | Se2—Nb3—Se12 | 136.91 (7) |
Se3i—Nb1—Se9 | 161.64 (7) | Se8—Nb3—Se12 | 75.26 (6) |
Se7—Nb1—Se9 | 86.89 (6) | Se1—Nb3—Se12 | 86.28 (6) |
Se4—Nb1—Se9 | 136.79 (6) | Se6—Nb3—Se12 | 122.37 (7) |
Se5—Nb1—Se9 | 100.10 (7) | Cl1—Nb3—Se10 | 83.72 (10) |
Se11—Nb1—Se9 | 50.60 (6) | Cl3—Nb3—Se10 | 84.67 (9) |
Cl2i—Nb1—Nb2 | 113.87 (9) | Se2—Nb3—Se10 | 163.19 (7) |
Cl4—Nb1—Nb2 | 130.60 (10) | Se8—Nb3—Se10 | 85.47 (6) |
Se3i—Nb1—Nb2 | 55.40 (4) | Se1—Nb3—Se10 | 137.10 (7) |
Se7—Nb1—Nb2 | 55.41 (4) | Se6—Nb3—Se10 | 98.36 (6) |
Se4—Nb1—Nb2 | 53.69 (4) | Se12—Nb3—Se10 | 50.84 (6) |
Se5—Nb1—Nb2 | 53.74 (5) | Cl1—Nb3—Nb2i | 114.40 (9) |
Se11—Nb1—Nb2 | 116.05 (6) | Cl3—Nb3—Nb2i | 132.36 (9) |
Se9—Nb1—Nb2 | 141.80 (6) | Se2—Nb3—Nb2i | 55.50 (5) |
Se4—Nb2—Se1i | 130.35 (6) | Se8—Nb3—Nb2i | 54.91 (4) |
Se4—Nb2—Se5 | 108.13 (6) | Se1—Nb3—Nb2i | 53.77 (4) |
Se1i—Nb2—Se5 | 93.89 (6) | Se6—Nb3—Nb2i | 53.90 (5) |
Se4—Nb2—Se6i | 94.11 (6) | Se12—Nb3—Nb2i | 115.37 (6) |
Se1i—Nb2—Se6i | 108.18 (6) | Se10—Nb3—Nb2i | 139.80 (6) |
Se5—Nb2—Se6i | 125.99 (6) | Se2—Se1—Nb2i | 65.18 (5) |
Se4—Nb2—Se8i | 141.21 (6) | Se2—Se1—Nb3 | 62.07 (6) |
Se1i—Nb2—Se8i | 82.95 (6) | Nb2i—Se1—Nb3 | 72.37 (5) |
Se5—Nb2—Se8i | 84.95 (6) | Se1—Se2—Nb3 | 64.57 (5) |
Se6i—Nb2—Se8i | 51.53 (5) | Se1—Se2—Nb2i | 62.64 (6) |
Se4—Nb2—Se3i | 52.30 (5) | Nb3—Se2—Nb2i | 72.33 (5) |
Se1i—Nb2—Se3i | 86.97 (6) | Se4i—Se3—Nb1i | 64.28 (6) |
Se5—Nb2—Se3i | 86.11 (5) | Se4i—Se3—Nb2i | 62.53 (6) |
Se6i—Nb2—Se3i | 141.77 (7) | Nb1i—Se3—Nb2i | 72.39 (5) |
Se8i—Nb2—Se3i | 166.03 (6) | Se3i—Se4—Nb1 | 62.24 (5) |
Se4—Nb2—Se2i | 87.44 (6) | Se3i—Se4—Nb2 | 65.18 (5) |
Se1i—Nb2—Se2i | 52.18 (5) | Nb1—Se4—Nb2 | 72.65 (5) |
Se5—Nb2—Se2i | 141.73 (6) | Se7—Se5—Nb2 | 65.48 (6) |
Se6i—Nb2—Se2i | 85.83 (6) | Se7—Se5—Nb1 | 62.40 (6) |
Se8i—Nb2—Se2i | 104.79 (6) | Nb2—Se5—Nb1 | 71.73 (5) |
Se3i—Nb2—Se2i | 76.12 (5) | Se8—Se6—Nb2i | 64.74 (6) |
Se4—Nb2—Se7 | 82.68 (6) | Se8—Se6—Nb3 | 62.37 (5) |
Se1i—Nb2—Se7 | 141.10 (7) | Nb2i—Se6—Nb3 | 71.72 (5) |
Se5—Nb2—Se7 | 51.32 (5) | Se5—Se7—Nb1 | 65.58 (6) |
Se6i—Nb2—Se7 | 85.47 (6) | Se5—Se7—Nb2 | 63.21 (6) |
Se8i—Nb2—Se7 | 77.74 (6) | Nb1—Se7—Nb2 | 72.02 (5) |
Se3i—Nb2—Se7 | 104.75 (6) | Se6—Se8—Nb3 | 65.48 (6) |
Se2i—Nb2—Se7 | 166.32 (6) | Se6—Se8—Nb2i | 63.73 (6) |
Se4—Nb2—Nb3i | 126.02 (6) | Nb3—Se8—Nb2i | 72.45 (5) |
Se1i—Nb2—Nb3i | 53.85 (5) | Se11—Se9—Nb1i | 64.54 (6) |
Se5—Nb2—Nb3i | 125.82 (5) | Nb1i—Se9—Nb1 | 89.66 (8) |
Se6i—Nb2—Nb3i | 54.38 (4) | Se12—Se10—Nb3 | 64.01 (6) |
Se8i—Nb2—Nb3i | 52.64 (4) | Nb3—Se10—Nb3ii | 89.82 (8) |
Se3i—Nb2—Nb3i | 126.88 (5) | Se9—Se11—Nb1 | 64.86 (6) |
Se2i—Nb2—Nb3i | 52.17 (4) | Nb1—Se11—Nb1i | 89.97 (8) |
Se7—Nb2—Nb3i | 128.36 (5) | Se10—Se12—Nb3ii | 65.15 (6) |
Se4—Nb2—Nb1 | 53.67 (5) | Nb3ii—Se12—Nb3 | 90.91 (8) |
Se1i—Nb2—Nb1 | 125.52 (6) | Nb3ii—Cl3—Nb3 | 96.62 (15) |
Se5—Nb2—Nb1 | 54.53 (4) | Nb1i—Cl4—Nb1 | 96.85 (17) |
Se6i—Nb2—Nb1 | 126.27 (5) | | |
Symmetry codes: (i) x, −y+1/2, z; (ii) x, −y+3/2, z. |
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