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The structure of the six-coordinate title complex, [YbI3(C4H8O)3], is the first mer-octa­hedral form of an LnI3L3 lanthanide (Ln) compound with neutral L ligands, and is closely related to that of several of the seven-coordinate LnX3L4 series of compounds, where X = Cl, Br or I and L = tetra­hydro­furan (THF), isopropanol, pyridine or water. A structural trans effect can be assigned to YbI3(THF)3, in contrast to the LnX3L4 compounds, where steric and crystal packing effects are significant. The Yb—I bond lengths are 2.9543 (4) and 2.9151 (6) Å for I trans and cis to I, respectively, and the Yb—O bond lengths are 2.299 (5) and 2.251 (3) Å for O trans and cis to I, respectively. The crystal packing allows for six contact distances as weak C—H...I inter­actions in the range 3.10–3.24 Å. The title molecule has a crystallographic twofold axis passing through a THF O atom, the trans I atom and the Yb atom.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270109038268/gg3217sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270109038268/gg3217Isup2.hkl
Contains datablock I

CCDC reference: 760057

Comment top

The crystal structures of many lanthanide (Ln) halide (X) compounds with one or more neutral ligands (L) are well known. For compounds with X=Cl, Br or I and small to moderate size neutral Lewis base ligands like tetrahydrofuran (THF), 1,2-dimethoxyethane (DME), pyradine (py), hexamethylphosphoramide [OP(NMe2)3], isopropyl alcohol (i-PrOH) and water (H2O), the most likely species to crystallize is the seven-coordinate LnXnL7-n. This situation is apparently the case whether the lanthanide is di- or tri-valent, where the number of neutral organic ligands is usually 5 or 4, respectively. Excluding LnX6 ions, there are only 18 six-coordinate monomeric LnX3L3 species with L as described above in the Cambridge Structural Database (CSD) to date (Version 5.30; Allen, 2002). However, the variety of Ln atom is not diminished, and the size of trivalent lanthanide radii appears to play no role in allowing octahedral coordination, as LnX3L3 compounds are observed with Ln = La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Yb and Lu and X = Cl, except for one X = Br compound, YbBr3(THF)3 (Deacon et al., 2000). Additionally, the organic ligands (L) may be small (e.g. H2O, py or THF) or large (e.g. triphenylarsine oxide; Ryan et al., 1987) and still yield a six-coordinate compound. This group of compounds includes the two LnX3(THF)3 analogs most closely related to the title compound, where Ln, X = Lu, Br (Magomedov et al., 1992) or Yb, Cl (Deacon et al., 1993).

For the six-coordinate LnX3L3 compounds, both fac and mer isomers are found in the CSD for X = Cl, but only mer isomers are found for X = Br, presumably as a result of the increased size of the bromide ion compared with the chloride ion. The title compound is the only six-coordinate triiodo species of this type, and a trans influence on bond geometries is evident, as shown by the data in Table 2. Other mer-octahedral trihalides of this type with significant trans influence are mer-YbBr3(THF)3 (Deacon, et al., 2000) and mer-SmBr3[OP(NMe2)3]2THF (Asakura & Imamoto, 2001). Of the seven mer isomers, five are LnCl3L3mer-YbCl3(THF)3 (Chang-Tao et al., 1993), mer-LuCl3(THF)3 (Magomedov et al., 1992), mer-DyCl3[OP(NMe2)3]3 (Xing-Wang et al., 1987), mer-PrCl3[OP(NMe2)3]3 (Radonovich & Glick, 1973) and mer-YbCl3[OP(NMe2)3]3 (Hou et al., 1991) – and two are LnBr3L3mer-YbBr3(THF)3 and mer-SmBr3[OP(NMe2)3]2THF. The fac isomers of six-coordinate LnX3L3 usually have larger L ligands, as in fac-trichlorido-tris(3-bromo-4-methoxylutidine N-oxide-O)praseodymium (Ban-Oganowska et al., 2002), fac-trichlorido-tris(triphenylarsine oxide)cerium (Ryan et al., 1987), fac-trichlorido-tris(2,6-dimethyl-4-pyrone)gadolinium (Bisi Castellani & Tazzoli, 1984), fac-trichlorido-tris(hexamethylphosphoramide-O)samarium (Petricek et al., 2000), fac-trichlorido-caprolactonato-O–bis(tetrahydrofuran)ytterbium (Evans et al., 1995) and fac-trichlorido-tris[bis(diethylamido)trichloroacetylamidophosphoric acid]praseodymium (Amirkhanov et al., 1995). Instances of fac LnCl3[OP(NMe2)3]3 are also known, namely, the isostructural series Ln = La, Pr, Sm, Eu, Nd and Gd (Petricek et al. 2000). The only instance of a seven-coordinate Ln3X3 compound approximating a fac isomer is when the sterically constrained tripodal ligand tris(2-pyridylmethyl)amine is used in a Ce triiodo complex (Natrajan et al., 2005).

When the DME bidentate ligand is used, the seven-coordinate compound is most likely to be produced, and there are over 80 instances in the CSD of LnX3Y4, where Y is the binding O atom (or N atom for di-, tri- or tetraamine) of a bidentate organic ligand. Unlike the Ce compound mentioned above, about 20 are of the type LnX3(DME)2 with X = Cl or Br only. There is one other LnI3Y4, where Y are O atoms from a multidentate ligand, namely, L = tetraglyme (Vestergren et al., 2004). In a broad sense, the nine compounds in the CSD of the type LnI3L4, where L are not multidentate, approximate the mer conformation (namely, having one nearly linear I—Ln—I angle and two ~90° I—Ln—I angles), even though there is seven-coordinate binding. This situation is presumably also due to the large volume occupied by each iodide ligand and to the fact that two I atoms are axial in the pentagonal–bipyramidal LnI3L4 complexes.

In the search for LnI3(Y = O,N)n species, the CSD revealed no six-coordinate, one nine-coordinate, five eight-coordinate and ten seven-coordinate compounds, with five compounds having tripodal ligands. For LnI3Ln and LnBr3Ln, neither L = py nor L = H2O species are found in the CSD. There are four LnI3(THF)4 compounds in the CSD; their Ln—I and Ln—O distances are compared with those of the title compound in Table 3, which shows a persistent trans influence on the O atom of the two THF ligands furthest from the equatorial I atom (the other two I atoms are trans to each other). However, as seven-coordinate pentagonal–bipyramidal compounds with five equatorial ligands, these LnI3(THF)4 compounds appear to have geometries significantly influenced by steric effects, especially with respect to the equatorial I ligand, such that the cis (e.g. equatorial) Ln—I bond is about 0.06 Å longer than either of the trans Ln—I bonds.

For LnBr3(O,N)n compounds, there are 11 seven-coordinate, one six-coordinate and one eight-coordinate species in the CSD, with five having tripodal ligands. Of these, one is YbBr3(THF)3 (Deacon et al., 2000) and four are LnBr3(THF)4. Details of their lanthanide bond geometries, as well as those of SmBr3(i-PrOH)4 (Depero et al., 1991) and NdBr3(THF)2(i-PrOH)2 (with THF ligands nearly trans to the equatorial Br atom; Ye Sun Chun et al., 1994), are also compared with the Yb—I and Yb—O bonds of the title YbI3(THF)3 compound in Table 3. There are many instances of LnCl3L3 and LnCl3L4, so bond comparisons here will be restricted to only L = THF, py and H2O, the smallest ligands in the series, and these compounds are included in Table 3.

For lanthanides with coordination saturated with halogens, only the LnX6 ions are found in the CSD. For LnX6, the range of Ln—X bonds for any Ln and X is about ±0.02Å from the average, which is not very narrow, even though these compounds are simple octahedra, indicating the likelihood of short-range nonsymmetrical crystal packing effects. There is one reported X = Br species, EuBr6, and the Eu—Br bonds are 2.80 (2) Å (Pellens et al., 2008); there are seven LnI6 [Ln = La, Pr, Nd (three examples), Sm and Er] with La—I bonds of 3.16 (2) Å (Babai & Mudring, 2006a), Pr—I bonds of 3.13 (2) Å (Babai &Mudring, 2005b), Nd—I bonds of 3.11 (2) Å (Babai &Mudring, 2005a; Babai & Mudring, 2006b), Sm—I bonds of 3.09 (2) Å (Babai &Mudring, 2005a) and Er—I bonds of 3.03 (1) Å (Babai &Mudring, 2006a); and there are 35 LnCl6 with an overall average Ln—Cl bond of 2.68 (2) Å and a range of 2.51–2.89 for the entire Ln series, but with a similar 0.01–0.03 Å variation from the mean for any given compound.

In summary, the YbI3(THF)3 complex reported here is the first instance of a six-coordinate triiodolanthanide. In addition, the observed mer conformation allows for the possibility of a trans influence which is rarely seen in six-coordinate lanthanide compounds. The bonds affected are the Yb—I and Yb—O bonds, which are 0.03 and 0.05 Å longer when trans to an I atom. Finally, six H···I contact distances in the range 3.10 to 3.24 Å are observed (Table 1), which are thus of the order of the van der Waals radii sum of 3.18 Å (Bondi, 1964). Although these distances are consistent with weak hydrogen-bond interactions, the THF ligand is traditionally expected to be a poor hydrogen-bond donor.

Related literature top

For related literature, see: Allen (2002); Amirkhanov et al. (1995); Asakura & Imamoto (2001); Babai & Mudring (2005a, 2005b, 2006a, 2006b); Ban-Oganowska, Godlewska, Macalik, Waskowska, Hanuza, Oganowski & Legendziewicz (2002); Bondi (1964); Bisi Castellani & Tazzoli (1984); Chang-Tao, Bing, Dao-Li, Cheng, Xiu-Ying, Rong-Guo & Huaxue (1993); Deacon et al. (1993, 2000); Depero et al. (1991); Evans et al. (1995); Hou et al. (1991); Kornienko et al. (2005); Magomedov et al. (1992); Natrajan et al. (2005); Pellens et al. (2008); Petricek et al. (2000); Radonovich & Glick (1973); Ryan et al. (1987); Vestergren et al. (2004); Xing-Wang, Xing-Fu, Benetollo & Bombieri (1987); Ye Sun Chun, Huang, Xian Xu, Sheng Ma & Shi (1994).

Experimental top

All syntheses were carried out under ultra pure nitrogen (JWS), using conventional dry-box or Schlenk techniques. Solvents (Fisher) were refluxed continuously over molten alkali metals or K/benzophenone and were collected immediately prior to use. Yb was purchased from Strom. Diphenyl diselenide (PhSeSePh) was purchased from Aldrich and recrystallized from hexane. For the synthesis of the title compound, Yb (2.0 mmol), PhSeSePh (2.0 mmol), iodine (1.0 mmol) and Hg (0.25 mmol) were combined in THF (50 ml). The mixture was stirred until all the metal was consumed. To the resulting yellow solution, elemental S (2.0 mmol) was added. After 24 h, the yellow solution was filtered and layered with hexanes (15 ml) to give yellow crystals. This procedure was originally designed to yield the Yb analog of an Er `double-cubane' cluster compound, (THF)10Er6S6I6.6(THF) (Kornienko et al., 2005).

Refinement top

All H atoms were located in difference Fourier maps and then treated as riding atoms. H atoms bonded to the THF C atoms were allowed to ride in geometrically idealized positions, with C—H = 0.99Å (CH2), with Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2009).

Figures top
[Figure 1] Fig. 1. : The molecular structure of YbI3(THF)3, with displacement ellipsoids drawn at the 50% probability level.
triiodidotris(tetrahydrofuran-κO)ytterbium(III) top
Crystal data top
[YbI3(C4H8O)3]F(000) = 1396
Mr = 770.05Dx = 2.614 Mg m3
Orthorhombic, PbcnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2abCell parameters from 3829 reflections
a = 9.3507 (7) Åθ = 2.6–30.5°
b = 14.6003 (11) ŵ = 9.51 mm1
c = 14.3335 (11) ÅT = 100 K
V = 1956.9 (3) Å3Lathe, yellow
Z = 40.20 × 0.20 × 0.10 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
2402 independent reflections
Radiation source: fine-focus sealed tube1808 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
phi and ω scansθmax = 28.3°, θmin = 2.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2003)
h = 128
Tmin = 0.22, Tmax = 0.41k = 1919
8941 measured reflectionsl = 1319
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.066H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.030P)2]
where P = (Fo2 + 2Fc2)/3
2402 reflections(Δ/σ)max < 0.001
88 parametersΔρmax = 1.35 e Å3
0 restraintsΔρmin = 0.74 e Å3
Crystal data top
[YbI3(C4H8O)3]V = 1956.9 (3) Å3
Mr = 770.05Z = 4
Orthorhombic, PbcnMo Kα radiation
a = 9.3507 (7) ŵ = 9.51 mm1
b = 14.6003 (11) ÅT = 100 K
c = 14.3335 (11) Å0.20 × 0.20 × 0.10 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
2402 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2003)
1808 reflections with I > 2σ(I)
Tmin = 0.22, Tmax = 0.41Rint = 0.037
8941 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0290 restraints
wR(F2) = 0.066H-atom parameters constrained
S = 1.00Δρmax = 1.35 e Å3
2402 reflectionsΔρmin = 0.74 e Å3
88 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) 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. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Yb10.00000.13361 (2)0.25000.01766 (9)
I10.19169 (4)0.12839 (3)0.08624 (2)0.02774 (10)
I20.00000.33327 (3)0.25000.02725 (12)
O10.1890 (4)0.1150 (3)0.1546 (2)0.0261 (8)
C10.2094 (6)0.1554 (5)0.0633 (4)0.0371 (16)
H1A0.20440.22300.06720.045*
H1B0.13450.13380.01960.045*
C20.3561 (6)0.1253 (4)0.0299 (4)0.0296 (12)
H2A0.35190.10360.03550.035*
H2B0.42540.17640.03400.035*
C30.3971 (6)0.0498 (5)0.0936 (5)0.0398 (15)
H3A0.37610.01020.06440.048*
H3B0.50060.05270.10760.048*
C40.3156 (8)0.0604 (6)0.1775 (5)0.060 (3)
H4A0.37350.09180.22570.072*
H4B0.28670.00030.20190.072*
O20.00000.0239 (3)0.25000.0302 (12)
C50.0136 (11)0.0832 (4)0.3306 (4)0.065 (3)
H5A0.11130.07880.35680.078*
H5B0.05560.06490.37940.078*
C60.0148 (11)0.1756 (5)0.3001 (6)0.068 (3)
H6A0.11560.19250.31240.081*
H6B0.04830.21960.33290.081*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Yb10.02106 (15)0.01552 (15)0.01640 (14)0.0000.00386 (11)0.000
I10.02805 (18)0.03006 (19)0.02512 (17)0.00554 (16)0.00445 (14)0.00095 (16)
I20.0365 (3)0.0165 (2)0.0287 (3)0.0000.0038 (2)0.000
O10.0257 (19)0.032 (2)0.0209 (18)0.0111 (17)0.0092 (15)0.0063 (16)
C10.027 (3)0.063 (5)0.021 (3)0.009 (3)0.009 (2)0.009 (3)
C20.029 (3)0.034 (3)0.026 (3)0.008 (3)0.013 (2)0.004 (3)
C30.024 (3)0.047 (4)0.048 (4)0.008 (3)0.008 (3)0.014 (3)
C40.054 (5)0.078 (6)0.049 (4)0.049 (4)0.025 (4)0.032 (4)
O20.055 (4)0.017 (3)0.019 (2)0.0000.006 (3)0.000
C50.147 (8)0.025 (3)0.022 (3)0.009 (4)0.001 (4)0.005 (2)
C60.118 (7)0.021 (3)0.065 (5)0.015 (4)0.035 (5)0.016 (3)
Geometric parameters (Å, º) top
Yb1—I12.9543 (4)C3—C41.432 (9)
Yb1—I22.9151 (6)C3—H3A0.9900
Yb1—O12.251 (3)C3—H3B0.9900
Yb1—O22.299 (5)C4—H4A0.9900
Yb1—O1i2.251 (3)C4—H4B0.9900
Yb1—I1i2.9543 (4)O2—C5i1.449 (7)
O1—C11.448 (6)O2—C51.449 (7)
O1—C41.465 (7)C5—C61.443 (10)
C1—C21.518 (8)C5—H5A0.9900
C1—H1A0.9900C5—H5B0.9900
C1—H1B0.9900C6—C6i1.464 (15)
C2—C31.482 (8)C6—H6A0.9900
C2—H2A0.9900C6—H6B0.9900
C2—H2B0.9900
I1—Yb1—I1i177.044 (18)H2A—C2—H2B108.9
I1—Yb1—I291.478 (9)C4—C3—C2107.4 (5)
O2—Yb1—I2180.0C4—C3—H3A110.2
O1i—Yb1—O1166.1 (2)C2—C3—H3A110.2
O1i—Yb1—O283.07 (10)C4—C3—H3B110.2
O1—Yb1—O283.07 (10)C2—C3—H3B110.2
O1i—Yb1—I296.93 (10)H3A—C3—H3B108.5
O1—Yb1—I296.93 (10)C3—C4—O1107.5 (5)
O1i—Yb1—I190.19 (10)C3—C4—H4A110.2
O1—Yb1—I189.46 (10)O1—C4—H4A110.2
O2—Yb1—I188.522 (9)C3—C4—H4B110.2
O1i—Yb1—I1i89.46 (10)O1—C4—H4B110.2
O1—Yb1—I1i90.19 (10)H4A—C4—H4B108.5
O2—Yb1—I1i88.522 (9)C5i—O2—C5106.6 (6)
I2—Yb1—I1i91.478 (9)C5i—O2—Yb1126.7 (3)
C1—O1—C4108.5 (4)C5—O2—Yb1126.7 (3)
C1—O1—Yb1127.1 (3)C6—C5—O2107.6 (6)
C4—O1—Yb1124.3 (3)C6—C5—H5A110.2
O1—C1—C2106.6 (4)O2—C5—H5A110.2
O1—C1—H1A110.4C6—C5—H5B110.2
C2—C1—H1A110.4O2—C5—H5B110.2
O1—C1—H1B110.4H5A—C5—H5B108.5
C2—C1—H1B110.4C5—C6—C6i105.2 (4)
H1A—C1—H1B108.6C5—C6—H6A110.7
C3—C2—C1104.7 (5)C6i—C6—H6A110.7
C3—C2—H2A110.8C5—C6—H6B110.7
C1—C2—H2A110.8C6i—C6—H6B110.7
C3—C2—H2B110.8H6A—C6—H6B108.8
C1—C2—H2B110.8
O1i—Yb1—O1—C1127.3 (5)C2—C3—C4—O122.3 (9)
O2—Yb1—O1—C1127.3 (5)C1—O1—C4—C313.1 (9)
I2—Yb1—O1—C152.7 (5)Yb1—O1—C4—C3168.4 (4)
I1—Yb1—O1—C138.7 (5)O1i—Yb1—O2—C5i121.4 (5)
I1i—Yb1—O1—C1144.2 (5)O1—Yb1—O2—C5i58.6 (5)
O1i—Yb1—O1—C454.5 (6)I1—Yb1—O2—C5i31.1 (5)
O2—Yb1—O1—C454.5 (6)I1i—Yb1—O2—C5i148.9 (5)
I2—Yb1—O1—C4125.5 (6)O1i—Yb1—O2—C558.6 (5)
I1—Yb1—O1—C4143.1 (6)O1—Yb1—O2—C5121.4 (5)
I1i—Yb1—O1—C434.0 (6)I1—Yb1—O2—C5148.9 (5)
C4—O1—C1—C21.0 (7)I1i—Yb1—O2—C531.1 (5)
Yb1—O1—C1—C2177.4 (4)C5i—O2—C5—C69.0 (5)
O1—C1—C2—C314.1 (7)Yb1—O2—C5—C6171.0 (5)
C1—C2—C3—C422.4 (8)O2—C5—C6—C6i23.3 (13)
Symmetry code: (i) x, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1A···I1ii0.993.243.926 (6)128
C1—H1B···I10.993.203.785 (6)120
C3—H3B···I1iii0.993.104.014 (6)155
C4—H4A···I1i0.993.233.715 (8)112
C4—H4B···I2iv0.993.223.879 (7)126
C5—H5A···I1i0.993.223.706 (7)112
Symmetry codes: (i) x, y, z+1/2; (ii) x+1/2, y+1/2, z; (iii) x+1, y, z; (iv) x+1/2, y1/2, z+1/2.

Experimental details

Crystal data
Chemical formula[YbI3(C4H8O)3]
Mr770.05
Crystal system, space groupOrthorhombic, Pbcn
Temperature (K)100
a, b, c (Å)9.3507 (7), 14.6003 (11), 14.3335 (11)
V3)1956.9 (3)
Z4
Radiation typeMo Kα
µ (mm1)9.51
Crystal size (mm)0.20 × 0.20 × 0.10
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2003)
Tmin, Tmax0.22, 0.41
No. of measured, independent and
observed [I > 2σ(I)] reflections
8941, 2402, 1808
Rint0.037
(sin θ/λ)max1)0.667
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.029, 0.066, 1.00
No. of reflections2402
No. of parameters88
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.35, 0.74

Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2009).

Selected geometric parameters (Å, º) top
Yb1—I12.9543 (4)Yb1—O12.251 (3)
Yb1—I22.9151 (6)Yb1—O22.299 (5)
I1—Yb1—I1i177.044 (18)O2—Yb1—I2180.0
I1—Yb1—I291.478 (9)O1i—Yb1—O1166.1 (2)
Symmetry code: (i) x, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1A···I1ii0.993.243.926 (6)128.0
C1—H1B···I10.993.203.785 (6)119.6
C3—H3B···I1iii0.993.104.014 (6)154.7
C4—H4A···I1i0.993.233.715 (8)111.8
C4—H4B···I2iv0.993.223.879 (7)125.6
C5—H5A···I1i0.993.223.706 (7)111.9
Symmetry codes: (i) x, y, z+1/2; (ii) x+1/2, y+1/2, z; (iii) x+1, y, z; (iv) x+1/2, y1/2, z+1/2.
Average Ln—X and Ln—Y trans to atom X or Y for LnX3L3 and LnX3L4, where X=I, Br, Cl; Y=O, N; L=THF, py, i-PrOH, H2O, O=P[N(Me2)]3. top
ave Ln-(I,Br or Cl) (Å)ave Ln-(O or N) (Å)neutral ligand, Lreference
7-coordinate compounds
La—I3.14/3.19La—O2.56/2.52THF(Trifonov et al., 1997)
Ce—I3.12/3.18Ce—O2.54/2.50THF(Liddle & Arnold, 2005)
Pr—I3.10/3.16Pr—O2.51/2.47THF(Izod et al., 2004)
Nd—I3.08/3.15Nd—O2.50/2.46THF(Balashova et al., 2007)
La—I3.20/3.21La—O2.51/2.51i-PrOH(Barnhart et al., 1995)
Ce—I3.17/3.19Ce—O2.48/2.49i-PrOH(Barnhart et al., 1995)
La—Br2.90/2.90La—O2.55/2.51THF(Deacon et al., 2000)
Ce—Br2.88/2.91Ce—O2.55/2.50THF(Hitchcock et al., 2004)
Pr—Br2.87/2.90Pr—O2.53/2.49THF(Petricek, 2004)
Sm—Br2.82/2.86Sm—O2.49/2.44THF(Petricek, 2004)
Nd—Br2.85/2.83Nd—O2.52/2.45THF,i-PrOH(Ye Sun Chun, et al., 1994)
Sm—Br2.85/2.80Sm—O2.49/2.43i-PrOH(Depero et al., 1991)
Eu—Cl2.62/2.64Eu—O2.47/2.45THF(De-Yuan, et al., 1998)
Gd—Cl2.62/2.66Gd—O2.46/2.48THF(Willey et al., 1997)
Sm—Cl2.68/2.68Sm—O2.49/2.45THF(Guan-Yang, et al., 1992)
Nd—Cl2.67/2.67Nd—O2.52/2.48THF(Wenqi et al., 1987)
La—Cl2.66/2.68La—N2.62/2.59py(Li et al., 2002)
Eu—Cl2.64/2.67Eu—N2.61/2.59py(Ning-Hai, et al., 1986)
Er—Cl2.58/2.62Er—N2.54/2.50py(Li et al., 2002)
Yb—Cl2.56/2.60Yb—N2.51/2.49py(Deacon et al., 2006)
Er—Cl2.60/2.66Er—O2.37/2.32H2O(Hines et al., 2008)
Tm—Cl2.64/2.62Tm—O2.35/2.35H2O(Semenova et al., 2006)
Yb—Cl2.63/2.62Yb—O2.33/2.26H2O(Semenova et al., 2006)
Lu—Cl2.59/2.60Lu—O2.35/2.28H2O(Semenova et al., 2006)
Er—Cl2.64/2.63Er—O2.35/2.29H2O(Semenova et al., 2006)
6-coordinate compounds
Yb—I2.95/2.92Yb—O2.30/2.25THFcurrent work
Yb—Br2.71/2.66Yb—O2.33/2.26THF(Deacon et al., 2000)
Sm—Br2.85/2.82Sm—O2.47/2.28THF(Asakura & Imamoto, 2001)
Yb—Cl2.53/2.51Yb—O2.36/2.27THF(Chang-Tao, et al., 1993)
Lu—Cl2.53/2.50Lu—O2.32/2.27THF(Magomedov et al., 1992)
Dy—Cl2.73/2.71Dy—O2.35/2.35i-PrOH(Radonovich & Glick, 1973)
Yb—Cl2.59/2.58Yb—O2.22/2.23i-PrOH(Hou et al., 1991)
 

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