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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806056364/mg2013sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806056364/mg2013Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](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

Computing details top

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
Nb3Se10Cl3F(000) = 2056
Mr = 1174.68Dx = 4.844 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 10764 reflections
a = 7.207 (3) Åθ = 3.0–27.5°
b = 18.974 (8) ŵ = 25.17 mm1
c = 11.834 (7) ÅT = 150 K
β = 95.60 (2)°Needle, black
V = 1610.6 (14) Å30.30 × 0.10 × 0.05 mm
Z = 4
Data collection top
Rigaku R-AXIS Rapid
diffractometer
2794 reflections with I > 2σ(I)
ω scansRint = 0.080
Absorption correction: numerical
(NUMABS; Higashi, 2000)
θmax = 27.5°, θmin = 3.0°
Tmin = 0.053, Tmax = 0.278h = 99
15892 measured reflectionsk = 2324
3799 independent reflectionsl = 1515
Refinement top
Refinement on F2154 parameters
Least-squares matrix: full0 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 = 1.07Δρmax = 3.51 e Å3
3799 reflectionsΔρmin = 2.66 e Å3
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
xyzUiso*/Ueq
Nb10.14692 (15)0.14950 (5)0.15458 (9)0.0163 (2)
Nb20.24186 (15)0.00022 (5)0.25164 (9)0.0166 (2)
Nb30.33033 (15)0.64911 (5)0.34990 (9)0.0164 (2)
Se10.02939 (17)0.61199 (7)0.21969 (11)0.0215 (3)
Se20.06429 (18)0.56996 (7)0.40624 (11)0.0227 (3)
Se30.07300 (18)0.42588 (7)0.26403 (12)0.0226 (3)
Se40.19677 (18)0.11482 (7)0.36995 (11)0.0217 (3)
Se50.21090 (19)0.03467 (7)0.03457 (11)0.0240 (3)
Se60.55234 (18)0.53713 (7)0.37425 (12)0.0255 (3)
Se70.46162 (18)0.08523 (7)0.14088 (12)0.0249 (3)
Se80.50649 (19)0.58792 (7)0.19658 (12)0.0245 (3)
Se90.2741 (3)0.250.01955 (16)0.0231 (4)
Se100.5968 (2)0.750.34996 (17)0.0236 (4)
Se110.4065 (2)0.250.20525 (16)0.0221 (4)
Se120.3732 (3)0.750.19538 (16)0.0223 (4)
Cl10.4090 (5)0.65224 (18)0.5597 (3)0.0282 (7)
Cl20.1323 (4)0.34744 (17)0.0121 (3)0.0275 (7)
Cl30.1212 (6)0.750.4059 (4)0.0215 (9)
Cl40.0371 (6)0.250.2331 (4)0.0231 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.0214 (5)0.0136 (5)0.0135 (5)0.0002 (4)0.0000 (4)0.0010 (4)
Nb20.0208 (5)0.0151 (5)0.0138 (5)0.0008 (5)0.0013 (4)0.0012 (4)
Nb30.0210 (5)0.0137 (5)0.0144 (5)0.0005 (4)0.0005 (4)0.0007 (4)
Se10.0217 (6)0.0214 (6)0.0206 (7)0.0016 (5)0.0013 (5)0.0018 (5)
Se20.0280 (6)0.0214 (6)0.0196 (7)0.0028 (5)0.0064 (5)0.0045 (5)
Se30.0230 (6)0.0213 (6)0.0238 (7)0.0007 (5)0.0047 (5)0.0038 (5)
Se40.0284 (6)0.0211 (6)0.0154 (6)0.0005 (5)0.0017 (5)0.0002 (5)
Se50.0309 (7)0.0241 (6)0.0166 (7)0.0018 (6)0.0015 (5)0.0008 (5)
Se60.0252 (6)0.0238 (7)0.0263 (7)0.0034 (6)0.0034 (5)0.0038 (5)
Se70.0250 (6)0.0202 (6)0.0302 (8)0.0002 (5)0.0061 (5)0.0041 (6)
Se80.0297 (7)0.0204 (6)0.0249 (7)0.0039 (6)0.0098 (5)0.0034 (5)
Se90.0324 (9)0.0209 (9)0.0168 (9)00.0058 (7)0
Se100.0214 (8)0.0208 (9)0.0284 (10)00.0004 (8)0
Se110.0230 (9)0.0206 (9)0.0222 (10)00.0010 (7)0
Se120.0285 (9)0.0217 (9)0.0168 (9)00.0030 (7)0
Cl10.0351 (17)0.0310 (17)0.0176 (16)0.0026 (15)0.0019 (13)0.0001 (13)
Cl20.0289 (15)0.0292 (16)0.0231 (17)0.0013 (14)0.0053 (13)0.0014 (14)
Cl30.0210 (19)0.0175 (19)0.026 (2)00.0046 (17)0
Cl40.033 (2)0.0147 (19)0.022 (2)00.0052 (18)0
Geometric parameters (Å, º) top
Nb1—Cl2i2.497 (3)Nb3—Cl12.492 (4)
Nb1—Cl42.549 (3)Nb3—Cl32.563 (3)
Nb1—Se3i2.5761 (19)Nb3—Se22.5741 (18)
Nb1—Se72.5942 (19)Nb3—Se82.589 (2)
Nb1—Se42.623 (2)Nb3—Se12.6311 (19)
Nb1—Se52.6654 (19)Nb3—Se62.6586 (19)
Nb1—Se112.6975 (18)Nb3—Se122.686 (2)
Nb1—Se92.7047 (19)Nb3—Se102.7114 (19)
Nb2—Se42.6234 (19)Nb1—Nb23.1075 (18)
Nb2—Se1i2.6283 (18)Nb2—Nb3i3.1053 (19)
Nb2—Se52.639 (2)Se1—Se22.338 (2)
Nb2—Se6i2.6423 (19)Se3—Se4i2.339 (2)
Nb2—Se8i2.6649 (18)Se5—Se72.308 (2)
Nb2—Se3i2.6837 (19)Se6—Se82.307 (2)
Nb2—Se2i2.6861 (19)Se9—Se112.309 (3)
Nb2—Se72.6895 (19)Se10—Se122.317 (3)
Cl2i—Nb1—Cl479.34 (13)Se8i—Nb2—Nb1128.22 (6)
Cl2i—Nb1—Se3i81.81 (10)Se3i—Nb2—Nb152.20 (4)
Cl4—Nb1—Se3i82.23 (9)Se2i—Nb2—Nb1126.96 (5)
Cl2i—Nb1—Se7128.37 (10)Se7—Nb2—Nb152.57 (4)
Cl4—Nb1—Se7149.71 (11)Nb3i—Nb2—Nb1179.08 (5)
Se3i—Nb1—Se7110.80 (6)Cl1—Nb3—Cl378.87 (13)
Cl2i—Nb1—Se4133.39 (10)Cl1—Nb3—Se281.88 (9)
Cl4—Nb1—Se481.98 (11)Cl3—Nb3—Se284.09 (9)
Se3i—Nb1—Se453.47 (5)Cl1—Nb3—Se8128.99 (10)
Se7—Nb1—Se484.55 (6)Cl3—Nb3—Se8149.00 (11)
Cl2i—Nb1—Se580.16 (9)Se2—Nb3—Se8110.40 (6)
Cl4—Nb1—Se5158.25 (11)Cl1—Nb3—Se1133.16 (10)
Se3i—Nb1—Se587.76 (6)Cl3—Nb3—Se183.07 (10)
Se7—Nb1—Se552.03 (5)Se2—Nb3—Se153.36 (5)
Se4—Nb1—Se5107.35 (6)Se8—Nb3—Se184.38 (6)
Cl2i—Nb1—Se11129.01 (9)Cl1—Nb3—Se680.51 (9)
Cl4—Nb1—Se1176.37 (10)Cl3—Nb3—Se6158.70 (12)
Se3i—Nb1—Se11136.73 (7)Se2—Nb3—Se687.78 (6)
Se7—Nb1—Se1175.79 (6)Se8—Nb3—Se652.15 (5)
Se4—Nb1—Se1186.28 (6)Se1—Nb3—Se6107.61 (6)
Se5—Nb1—Se11122.96 (7)Cl1—Nb3—Se12129.12 (10)
Cl2i—Nb1—Se983.22 (10)Cl3—Nb3—Se1275.73 (10)
Cl4—Nb1—Se984.61 (10)Se2—Nb3—Se12136.91 (7)
Se3i—Nb1—Se9161.64 (7)Se8—Nb3—Se1275.26 (6)
Se7—Nb1—Se986.89 (6)Se1—Nb3—Se1286.28 (6)
Se4—Nb1—Se9136.79 (6)Se6—Nb3—Se12122.37 (7)
Se5—Nb1—Se9100.10 (7)Cl1—Nb3—Se1083.72 (10)
Se11—Nb1—Se950.60 (6)Cl3—Nb3—Se1084.67 (9)
Cl2i—Nb1—Nb2113.87 (9)Se2—Nb3—Se10163.19 (7)
Cl4—Nb1—Nb2130.60 (10)Se8—Nb3—Se1085.47 (6)
Se3i—Nb1—Nb255.40 (4)Se1—Nb3—Se10137.10 (7)
Se7—Nb1—Nb255.41 (4)Se6—Nb3—Se1098.36 (6)
Se4—Nb1—Nb253.69 (4)Se12—Nb3—Se1050.84 (6)
Se5—Nb1—Nb253.74 (5)Cl1—Nb3—Nb2i114.40 (9)
Se11—Nb1—Nb2116.05 (6)Cl3—Nb3—Nb2i132.36 (9)
Se9—Nb1—Nb2141.80 (6)Se2—Nb3—Nb2i55.50 (5)
Se4—Nb2—Se1i130.35 (6)Se8—Nb3—Nb2i54.91 (4)
Se4—Nb2—Se5108.13 (6)Se1—Nb3—Nb2i53.77 (4)
Se1i—Nb2—Se593.89 (6)Se6—Nb3—Nb2i53.90 (5)
Se4—Nb2—Se6i94.11 (6)Se12—Nb3—Nb2i115.37 (6)
Se1i—Nb2—Se6i108.18 (6)Se10—Nb3—Nb2i139.80 (6)
Se5—Nb2—Se6i125.99 (6)Se2—Se1—Nb2i65.18 (5)
Se4—Nb2—Se8i141.21 (6)Se2—Se1—Nb362.07 (6)
Se1i—Nb2—Se8i82.95 (6)Nb2i—Se1—Nb372.37 (5)
Se5—Nb2—Se8i84.95 (6)Se1—Se2—Nb364.57 (5)
Se6i—Nb2—Se8i51.53 (5)Se1—Se2—Nb2i62.64 (6)
Se4—Nb2—Se3i52.30 (5)Nb3—Se2—Nb2i72.33 (5)
Se1i—Nb2—Se3i86.97 (6)Se4i—Se3—Nb1i64.28 (6)
Se5—Nb2—Se3i86.11 (5)Se4i—Se3—Nb2i62.53 (6)
Se6i—Nb2—Se3i141.77 (7)Nb1i—Se3—Nb2i72.39 (5)
Se8i—Nb2—Se3i166.03 (6)Se3i—Se4—Nb162.24 (5)
Se4—Nb2—Se2i87.44 (6)Se3i—Se4—Nb265.18 (5)
Se1i—Nb2—Se2i52.18 (5)Nb1—Se4—Nb272.65 (5)
Se5—Nb2—Se2i141.73 (6)Se7—Se5—Nb265.48 (6)
Se6i—Nb2—Se2i85.83 (6)Se7—Se5—Nb162.40 (6)
Se8i—Nb2—Se2i104.79 (6)Nb2—Se5—Nb171.73 (5)
Se3i—Nb2—Se2i76.12 (5)Se8—Se6—Nb2i64.74 (6)
Se4—Nb2—Se782.68 (6)Se8—Se6—Nb362.37 (5)
Se1i—Nb2—Se7141.10 (7)Nb2i—Se6—Nb371.72 (5)
Se5—Nb2—Se751.32 (5)Se5—Se7—Nb165.58 (6)
Se6i—Nb2—Se785.47 (6)Se5—Se7—Nb263.21 (6)
Se8i—Nb2—Se777.74 (6)Nb1—Se7—Nb272.02 (5)
Se3i—Nb2—Se7104.75 (6)Se6—Se8—Nb365.48 (6)
Se2i—Nb2—Se7166.32 (6)Se6—Se8—Nb2i63.73 (6)
Se4—Nb2—Nb3i126.02 (6)Nb3—Se8—Nb2i72.45 (5)
Se1i—Nb2—Nb3i53.85 (5)Se11—Se9—Nb1i64.54 (6)
Se5—Nb2—Nb3i125.82 (5)Nb1i—Se9—Nb189.66 (8)
Se6i—Nb2—Nb3i54.38 (4)Se12—Se10—Nb364.01 (6)
Se8i—Nb2—Nb3i52.64 (4)Nb3—Se10—Nb3ii89.82 (8)
Se3i—Nb2—Nb3i126.88 (5)Se9—Se11—Nb164.86 (6)
Se2i—Nb2—Nb3i52.17 (4)Nb1—Se11—Nb1i89.97 (8)
Se7—Nb2—Nb3i128.36 (5)Se10—Se12—Nb3ii65.15 (6)
Se4—Nb2—Nb153.67 (5)Nb3ii—Se12—Nb390.91 (8)
Se1i—Nb2—Nb1125.52 (6)Nb3ii—Cl3—Nb396.62 (15)
Se5—Nb2—Nb154.53 (4)Nb1i—Cl4—Nb196.85 (17)
Se6i—Nb2—Nb1126.27 (5)
Symmetry codes: (i) x, y+1/2, z; (ii) x, y+3/2, z.
 

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