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NbF5 was synthesized in high purity by direct fluorination. IR and Raman spectroscopy confirms the high purity. The crystal structure was redetermined at 100 K with higher precision.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989023010150/ox2001sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989023010150/ox2001Isup2.hkl
Contains datablock I

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2056989023010150/ox2001Isup3.rtv
Contains datablock I

docx

Microsoft Word (DOCX) file https://doi.org/10.1107/S2056989023010150/ox2001sup4.docx
IR and Raman spectra

CCDC references: 2309973; 2289431

Computing details top

Niobium(V) fluoride top
Crystal data top
Nb4F20F(000) = 688
Mr = 187.91Dx = 3.719 Mg m3
Monoclinic, C2/mMo Kα radiation, λ = 0.71073 Å
a = 9.4863 (12) ÅCell parameters from 8094 reflections
b = 14.2969 (12) Åθ = 2.6–30.9°
c = 4.9892 (6) ŵ = 3.56 mm1
β = 97.292 (10)°T = 100 K
V = 671.19 (13) Å3Block, colorless
Z = 80.18 × 0.05 × 0.05 mm
Data collection top
Stoe IPDSII
diffractometer
1048 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus903 reflections with I > 2σ(I)
Detector resolution: 6.67 pixels mm-1Rint = 0.032
rotation method, ω scansθmax = 30.4°, θmin = 2.6°
Absorption correction: numerical
(X-RED32 and X-SHAPE; Stoe & Cie, Stoe & Cie, 2020)
h = 1313
Tmin = 0.776, Tmax = 0.778k = 1820
5819 measured reflectionsl = 77
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: dual
R[F2 > 2σ(F2)] = 0.014Secondary atom site location: difference Fourier map
wR(F2) = 0.032 w = 1/[σ2(Fo2) + (0.0196P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
1048 reflectionsΔρmax = 0.54 e Å3
60 parametersΔρmin = 0.52 e Å3
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
xyzUiso*/Ueq
Nb10.0000000.20347 (2)0.5000000.01085 (6)
Nb20.26047 (2)0.0000000.24168 (4)0.01094 (6)
F10.34193 (16)0.0000000.6005 (3)0.0169 (3)
F20.13043 (15)0.0000000.0646 (3)0.0148 (3)
F30.36790 (12)0.09599 (7)0.1443 (2)0.0179 (2)
F40.12213 (11)0.09546 (6)0.3786 (2)0.01482 (19)
F50.10961 (12)0.18505 (7)0.17107 (19)0.0163 (2)
F60.11939 (13)0.28718 (7)0.3733 (2)0.0171 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.01143 (11)0.00957 (9)0.01173 (9)0.0000.00212 (7)0.000
Nb20.01106 (10)0.01044 (9)0.01157 (10)0.0000.00242 (7)0.000
F10.0168 (7)0.0195 (6)0.0141 (6)0.0000.0011 (5)0.000
F20.0145 (6)0.0152 (6)0.0145 (6)0.0000.0013 (5)0.000
F30.0177 (5)0.0169 (5)0.0196 (5)0.0046 (4)0.0043 (4)0.0012 (4)
F40.0150 (4)0.0130 (4)0.0170 (4)0.0021 (4)0.0039 (3)0.0013 (4)
F50.0176 (5)0.0163 (4)0.0146 (4)0.0003 (4)0.0008 (4)0.0004 (4)
F60.0175 (5)0.0152 (4)0.0189 (5)0.0026 (4)0.0036 (4)0.0018 (4)
Geometric parameters (Å, º) top
Nb1—F61.8157 (11)Nb2—F31.8121 (10)
Nb1—F6i1.8158 (10)Nb2—F3ii1.8122 (10)
Nb1—F51.8468 (10)Nb2—F21.8378 (14)
Nb1—F5i1.8468 (10)Nb2—F11.8577 (14)
Nb1—F4i2.0669 (9)Nb2—F42.0685 (10)
Nb1—F42.0669 (9)Nb2—F4ii2.0685 (10)
F6—Nb1—F6i97.52 (7)F3—Nb2—F296.78 (5)
F6—Nb1—F595.18 (5)F3ii—Nb2—F296.78 (5)
F6i—Nb1—F595.61 (5)F3—Nb2—F194.53 (5)
F6—Nb1—F5i95.61 (5)F3ii—Nb2—F194.53 (5)
F6i—Nb1—F5i95.18 (5)F2—Nb2—F1162.63 (6)
F5—Nb1—F5i163.61 (7)F3—Nb2—F489.47 (5)
F6—Nb1—F4i172.83 (4)F3ii—Nb2—F4171.95 (4)
F6i—Nb1—F4i89.59 (4)F2—Nb2—F483.54 (5)
F5—Nb1—F4i83.14 (5)F1—Nb2—F483.43 (4)
F5i—Nb1—F4i84.63 (4)F3—Nb2—F4ii171.95 (4)
F6—Nb1—F489.59 (4)F3ii—Nb2—F4ii89.47 (5)
F6i—Nb1—F4172.83 (4)F2—Nb2—F4ii83.54 (5)
F5—Nb1—F484.62 (4)F1—Nb2—F4ii83.43 (4)
F5i—Nb1—F483.14 (5)F4—Nb2—F4ii82.57 (5)
F4i—Nb1—F483.32 (5)Nb1—F4—Nb2172.94 (5)
F3—Nb2—F3ii98.46 (7)
Symmetry codes: (i) x, y, z+1; (ii) x, y, z.
Selected crystallographic details for NbF5 determined from single crystal X-ray diffraction (SCXRD, middle column) and powder X-ray diffraction (PXRD, Rietveld refinement, right column) top
NbF5 (SCXRD)NbF5 (PXRD)
Empirical formulaNbF5NbF5
Empirical formula moietyNb4F20Nb4F20
Color and appearancecolorless blockcolorless powder
Size (mm3); capillary diameter (mm)0.180 × 0.050 × 0.0500.3
Molecular mass (g mol–1)187.91187.91
Crystal systemmonoclinicmonoclinic
Space group (No.)C2/m (12)C2/m (12)
Pearson symbolmC48mC48
a (Å)9.4863 (12)9.62749 (19)
b (Å)14.2969 (12)14.4564 (3)
c (Å)4.9892 (6)5.12831 (10)
β (°)97.292 (10)95.8243 (4)
V3)671.19 (13)710.07 (3)
Z88
Z'22
ρcalc (g cm-3)3.7193.515
λ (Å)0.71073 (Mo Kα)1.540596 (Cu Kα1)
T (K)100293
µ (mm-1)3.56127.9495
2θ range measured (min, max, increment)5.182, 60.76, –6.885, 80.340, 0.015
2θ range refined (min, max)10.005, 80.340
hklmax-13 h 130 h 8
-18 k 180 k 12
-7 l 7-4 l 4
Absorption correctionnumericalcylindrical
Tmax, Tmin0.7778, 0.7760
Rint, Rσ0.0318, 0.0172
Completeness0.994
No. of unique reflections1048240
No. of parameters6074
No. of restraints00
No. of constraints00
Background parameters20
Profile parameters12a
Rp, Rwp0.0308, 0.0425
Rpb, Rwpb0.0889, 0.0904
RBragg0.0132
S (all data)1.0241.77
R(F) [I 2σ(I), all data]0.0143, 0.0198
wR(F2) [I 2σ(I), all data]0.0315, 0.0323
Δρmax, Δρmin (e Å-3)0.544, –0.521
Notes: (a) refined profile parameters include spherical harmonics of order 4; (b) background-corrected R-factors.
Selected interatomic distances (Å) for the crystal structure of NbF5 top
Nb1—F42.0669 (9)Nb2—F31.8121 (10)
Nb1—F51.8468 (10)Nb2—F42.0685 (10)
Nb1—F61.8157 (11)Nb1—Nb24.1275 (4)
Nb2—F11.8577 (14)Nb1—Nb1iii5.8179 (6)
Nb2—F21.8378 (14)Nb2—Nb2ii5.8565 (8)
Symmetry codes: (i) x, -y, z; (ii) -x, y, 1 - z, (iii) -x, -y, 1 - z.
Selected interatomic angles (°) for the crystal structure of NbF5. top
F6—Nb1—F6ii97.52 (7)F3—Nb2—F3i98.46 (7)
F6—Nb1—F595.18 (5)F3—Nb2—F296.78 (5)
F6i—Nb1—F595.61 (5)F3i—Nb2—F296.78 (5)
F6—Nb1—F5ii95.61 (5)F3—Nb2—F194.53 (5)
F6ii—Nb1—F5ii95.18 (5)F3i—Nb2—F194.53 (5)
F5—Nb1—F5ii163.61 (7)F2—Nb2—F1162.63 (6)
F6—Nb1—F4ii172.83 (4)F3—Nb2—F489.47 (5)
F6ii—Nb1—F4ii89.59 (4)F3i—Nb2—F4171.95 (4)
F5—Nb1—F4ii83.14 (5)F2—Nb2—F483.54 (5)
F5ii—Nb1—F4ii84.63 (4)F1—Nb2—F483.43 (4)
F6—Nb1—F489.59 (4)F3—Nb2—F4i171.95 (4)
F6ii—Nb1—F4172.83 (4)F3i—Nb2—F4i89.47 (5)
F5—Nb1—F484.62 (4)F2—Nb2—F4i83.54 (5)
F5ii—Nb1—F483.14 (5)F1—Nb2—F4i83.43 (4)
F4ii—Nb1—F483.32 (5)F4—Nb2—F4i82.57 (5)
Nb1—Nb2—Nb1iii89.62 (1)Nb1—F4—Nb2172.94 (5)
Nb2—Nb1—Nb2ii90.38 (1)
Symmetry codes: (i) x, -y, z; (ii) -x, y, 1 - z, (iii) -x, -y, 1 - z.
Selected interatomic angles (°) for the crystal structure of NbF5 top
F6i—Nb1—F595.61 (5)F3i—Nb2—F296.78 (5)
F6—Nb1—F6ii97.52 (7)F3—Nb2—F3i98.46 (7)
F6—Nb1—F595.18 (5)F3—Nb2—F296.78 (5)
F6i—Nb1—F595.61 (5)F3i—Nb2—F296.78 (5)
F6—Nb1—F5ii95.61 (5)F3—Nb2—F194.53 (5)
F6ii—Nb1—F5ii95.18 (5)F3i—Nb2—F194.53 (5)
F5—Nb1—F5ii163.61 (7)F2—Nb2—F1162.63 (6)
F6—Nb1—F4ii172.83 (4)F3—Nb2—F489.47 (5)
F6ii—Nb1—F4ii89.59 (4)F3i—Nb2—F4171.95 (4)
F5—Nb1—F4ii83.14 (5)F2—Nb2—F483.54 (5)
F5ii—Nb1—F4ii84.63 (4)F1—Nb2—F483.43 (4)
F6—Nb1—F489.59 (4)F3—Nb2—F4i171.95 (4)
F6ii—Nb1—F4172.83 (4)F3i—Nb2—F4i89.47 (5)
F5—Nb1—F484.62 (4)F2—Nb2—F4i83.54 (5)
F5ii—Nb1—F483.14 (5)F1—Nb2—F4i83.43 (4)
F4ii—Nb1—F483.32 (5)F4—Nb2—F4i82.57 (5)
Nb1—Nb2—Nb1iii89.62 (1)Nb1—F4—Nb2172.94 (5)
Nb2—Nb1—Nb2ii90.38 (1)
Symmetry codes: (i) x, -y, z; (ii) -x, y, 1 - z, (iii) -x, -y, 1 - z.

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