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The crystal structure of hexa-μ-hydroxo-do­deca­methylocta-μ3-oxo-do­deca­gallium(III) bis­[tetra­kis­(penta­fluoro­phenyl)­borate(III)] chloro­benzene disolvate dihydrate, [Ga12(CH3)123-O)8(μ-OH)6](C24F20B)2·2C6H5Cl·2H2O, is reported. The gallium–oxo–hydroxide dication is located on an inversion center and adopts a cage structure composed of 12 fused Ga3O3 rings and is associated with the hydrate mol­ecules and the [B(C6F5)4] anions through hydrogen bonds and one O—H...π-ring interaction. Disordered chloro­benzene solvent mol­ecules are also present in the crystal structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100009902/fg1603sup1.cif
Contains datablocks global, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100009902/fg1603IIsup2.hkl
Contains datablock II

CCDC reference: 152601

Comment top

In recent reports, we have described the chemistry of novel cationic group 13 alkyl complexes, some of which polymerize ethylene (Coles & Jordan, 1997; Ihara et al., 1998; Radzewich et al., 1998, 1999; Korolev et al., 1999; Dagorne et al., 2000). In the course of these studies, we found that the dinuclear cationic Ga–amidinate complex [{tBuC(NiPr)2}GaMe2.{tBuC(NiPr)2}GaMe][B(C6F5)4], (I), is hydrolyzed to the unexpected dicationic gallium–oxo–hydroxide cage compound [Ga12Me123-O)8(µ-OH)6][B(C6F5)4]2 2H2O, (II). The molecular structure of (II) solvated with chlorobenzene is reported here.

Compound (II) crystallizes as [Ga12Me123-O)8(µ-OH)6]2+ dications (Fig. 1) that are associated with the hydrate molecules and the [B(C6F5)4] anions by hydrogen bonds and one O—H···π-ring interaction. Two chlorobenzene solvate molecules are also present in the crystal structure. The dication of (II) adopts a cage structure that is composed of 12 fused six-membered Ga3O3 rings and is positioned on a center of symmetry. Each Ga–Me unit is coordinated to two µ3-O atoms and one µ-OH group. The cage structure of the [Ga12Me123-O)8(µ-OH)6]2+ dication is very similar to that of the neutral gallium–oxo–hydroxide complex Ga12tBu123-O)8(µ-O)2(µ-OH)4 (Barron et al., 1995), which is a doubly deprotonated analogue of (II). The Ga centers in (II) exhibit slightly distorted tetrahedral geometries. The O—Ga—O bond angles [average 100 (3)°] are smaller than the ideal tetrahedral value, which is compensated for by an opening of the O—Ga—C bond angles [average 118 (3)°]. The Ga—(µ3-O) bond distances [average 1.87 (2) Å] are comparable to the Ga—O bond distances in gallium oxide (1.87–1.89 Å; Barron et al., 1995) and to the Ga—(µ3-O) distances in Ga12tBu123-O)8(µ-O)2(µ-OH)4 (1.878–1.915 Å; Barron et al., 1995) and Ga6Mes63-O)4(µ3-OH)4·6THF (Mes is mesityl; 1.855–1.896 Å; Roesky et al., 1994). The µ3-O centers exhibit trigonal–planar geometry. The Ga—(µ-OH) bond distances [average 1.92 (2) Å] are similar to those in the dinuclear Ga cation [(iPr2—ATI)GaMe]2(µ-OH)+ [1.941 (3) Å; Guzei et al., 2000] and the neutral Ga dimer [{CH(SiMe3)2}2Ga(µ-OH)]2 [average 1.96 (1) Å; Uhl et al., 1996]. The Ga—(µ-OH)—Ga bond angles [average 128.4 (8)°] are nearly identical to those in Ga12tBu123-O)8(µ-O)2(µ-OH)4 [average 129.1 (1) Å; Barron et al. 1995]. The Ga—C bond distances [average 1.92 (2) Å] in (II) are significantly shorter than those in Ga12tBu123-O)8(µ-O)2(µ-OH)4 [average 1.98 (1) Å] due to the difference in cluster charge (dication versus neutral) and alkyl group size (Me versus tBu). The Ga—C distances in (II) are also shorter than those in [(iPr2—ATI)GaMe]2(µ-OH)+ [1.941 (3) Å; Guzei et al., 2000] and (I) [average 1.950 (3) Å; Dagorne et al., 2000].

The hydrate molecules and the [B(C6F5)4] anions of (II) are hydrogen bonded to the [Ga12Me123-O)8(µ-OH)6]2+ dication through the Ga(µ-OH) groups. There are four unique hydrogen bonds (Table 2) and one O—H···π-ring interaction. The strongest interaction is between the O11—H11 group and the O90 water molecule, and can be considered as a moderate strength hydrogen bond (Jeffrey, 1997). Similar hydrogen bonds are present in Ga6Mes63-O)43-OH)4·6THF, in which the tetrahydrofuran molecules are hydrogen bonded to the µ3-OH group, and in Me2Ga(µ-OH)(µ-Me2Pz)GaMe2·HOCH2Me2pz (pz is pyrazolyl), in which the OH group of the HOCH2Me2pz molecule is hydrogen bonded to the µ-OH group (Roesky et al., 1994; Trotter et al., 1988). The second hydrogen bond in (II) is the O12—H12···F22 interaction which is longer than that in 2-fluoro-1,1,2-triphenyl ethanol [F···O = 2.73 (4) Å; Desmarteau et al., 1992]. The other two hydrogen bonds are from the O90 water H atoms to F atoms of the anion. Hydrogen bonds from O—H donors to organic C—F groups are not common and may be ascribed, in the present case, to the electrostatic attraction between the [Ga12Me123-O)8(µ-OH)6]2+ dication and the [B(C6F5)4] anions (Desiraju & Steiner, 1999). Additionally an O—H···π-ring interaction is present between the O13 H atom and the (C11–C16)i phenyl ring: H13···π-ring = 3.11 Å, O13—H13···π-ring centroid = 159° [the coordinates for the ring centroid are 0.30717, 0.56226, 0.14106; symmetry code: (i) 1 + x, y, z]

The [B(C6F5)4] anion in (II) adopts a slightly distorted tetrahedral structure. The C22—F22 bond distance is slightly longer than other C—F bond distances and may be due to the O12—H12—F22 hydrogen bond.

Experimental top

A mixture of [tBuC(NiPr)2]GaMe2 (200 mg, 0.706 mmol) and [Ph3C][[B(C6F5)4] (326 mg, 0.353 mmol) in benzene (1 ml) was stirred for 1 h at 296 K. The benzene was removed under vacuum and the resulting yellow oil was analyzed by 1H NMR (C6D5Cl), which established that (I) had formed quantitatively along with 0.5 equivalents of Ph3CMe (Dagorne et al., 2000). The solvent was removed under vacuum and the resulting oil was taken up in a 1:9 C6H5Cl–pentane solvent mixture (1 ml). The solution was stored at 243 K for 2 d, after which time, pale-yellow crystals of (II) had formed.

Refinement top

The chlorobenzene solvent molecule was disordered over two sites, with occupancies of 0.648 and 0.352 for the Cl atom. A rotatation of approximately 120° about an axis through the center and perpedicular to the plane of the benzene ring produces the second Cl-atom site from the first. Due to apparent high thermal motion, each site was modelled with two rigid groups (C—C = 1.4 Å, C—Cl = 1.74 Å, C—H = 0.95 Å, all angles = 120°) of partial and equal occupancy. Two group isotropic displacement parameters were used for the C atoms, one for each site. Anisotropic displacement parameters were used for the Cl atoms, with those in close proximity (i.e. of the same site) constrained to be the same. The O–H bonds of the water molecule were restrained to be 0.84 Å and the H···H intramolecular distance was restrained to be 1.33 Å. The hydroxyl and water H-atom locations were supported by difference-map peaks from SHELXL `omit' maps.

Computing details top

Data collection: CAD-4 Operations Manual (Enraf-Nonius, 1977); cell refinement: CAD-4 Operations Manual; data reduction: MolEN (Fair, 1990); program(s) used to solve structure: SHELXTL (Sheldrick, 1995); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The [Ga12Me123-O)8(µ-OH)6]2+ dication of (II). Displacement ellipsoids are shown at the 35% probability level.
(II) top
Crystal data top
[Ga12C12H42O14](C24F20B)2·2C6H5Cl·2H2OZ = 1
Mr = 2866.32F(000) = 1392
Triclinic, P1Dx = 1.938 Mg m3
a = 13.532 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 15.223 (5) ÅCell parameters from 40 reflections
c = 12.755 (3) Åθ = 11.2–14.9°
α = 101.98 (2)°µ = 3.42 mm1
β = 106.91 (2)°T = 210 K
γ = 83.71 (2)°Prism, pale yellow
V = 2455.7 (11) Å30.34 × 0.28 × 0.18 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
4561 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.073
Graphite monochromatorθmax = 25.0°, θmin = 2.0°
θ–2θ scansh = 1616
Absorption correction: ψ scans
(MolEN; Fair, 1990)
k = 1818
Tmin = 0.329, Tmax = 0.540l = 156
10851 measured reflections4 standard reflections every 120 min
8067 independent reflections intensity decay: 15.2%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.056H-atom parameters constrained
wR(F2) = 0.122 w = 1/[σ2(Fo2) + (0.0413P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max = 0.009
8067 reflectionsΔρmax = 0.55 e Å3
620 parametersΔρmin = 0.76 e Å3
3 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0029 (3)
Crystal data top
[Ga12C12H42O14](C24F20B)2·2C6H5Cl·2H2Oγ = 83.71 (2)°
Mr = 2866.32V = 2455.7 (11) Å3
Triclinic, P1Z = 1
a = 13.532 (3) ÅMo Kα radiation
b = 15.223 (5) ŵ = 3.42 mm1
c = 12.755 (3) ÅT = 210 K
α = 101.98 (2)°0.34 × 0.28 × 0.18 mm
β = 106.91 (2)°
Data collection top
Enraf-Nonius CAD-4
diffractometer
4561 reflections with I > 2σ(I)
Absorption correction: ψ scans
(MolEN; Fair, 1990)
Rint = 0.073
Tmin = 0.329, Tmax = 0.5404 standard reflections every 120 min
10851 measured reflections intensity decay: 15.2%
8067 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0563 restraints
wR(F2) = 0.122H-atom parameters constrained
S = 1.11Δρmax = 0.55 e Å3
8067 reflectionsΔρmin = 0.76 e Å3
620 parameters
Special details top

Experimental. During refinement of the data versus. the model, a number of poorly fitting data prompted a closer examination of the raw data. This led to the discovery of an intermittant electronic problem. A failing cable caused some data to be recorded with zero or near zero intensity. The faulty data were identified in two ways. First, an examination of equivalent reflections in poor agreement (one with zero intensity, the other significantly above zero) led to the rejection of approximately 400 redundant data. Second, when the refinement was near convergence, the F(obs) - F(calc) listing was checked for data with large negative values. These data were checked and those with a reflection profile characteristic of the problem (partially or totally flat) were removed (approximately 520 reflections) from the data set and the final refinement was completed with the corrected data set.

Geometry. Note: Two orientations for the chlorobenzene were found and due to high thermal motion each orientation was modelled with two rigid groups of equal occupancy and the same the thermal parameters. This model places site C135 within 3.11 Å of a symmetry equivalent position. The actual average position of the C atom in this orientation is approximated by the average of sites C125+C135. The same symmetry operation that gives a close contact for C135 gives a contact distance of 3.67 Å for the averaged site position (C125+C135).

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*/UeqOcc. (<1)
Ga10.02716 (6)0.61462 (7)0.72588 (8)0.0395 (3)
Ga20.12731 (6)0.68139 (7)0.49122 (8)0.0393 (3)
Ga30.00431 (6)0.60410 (7)0.31370 (8)0.0380 (3)
Ga40.12123 (6)0.67728 (7)0.57710 (8)0.0390 (3)
Ga50.21804 (6)0.48995 (7)0.46133 (8)0.0383 (3)
Ga60.19113 (6)0.51130 (7)0.70914 (8)0.0384 (3)
C10.0722 (7)0.6618 (7)0.8566 (7)0.059 (3)
H1A0.02860.70880.90250.088*
H1B0.06810.61460.89760.088*
H1C0.14240.68540.83530.088*
C20.1809 (7)0.8022 (6)0.5236 (9)0.068 (3)
H2A0.16860.83640.47370.103*
H2B0.14720.82860.59910.103*
H2C0.25400.80240.51410.103*
C30.0387 (7)0.6729 (6)0.2004 (9)0.061 (3)
H3A0.10130.65030.14780.091*
H3B0.01420.66890.16300.091*
H3C0.05110.73450.23240.091*
C40.2086 (6)0.7753 (6)0.5933 (7)0.049 (2)
H4A0.26060.78020.66360.074*
H4B0.16710.83050.59050.074*
H4C0.24120.76350.53390.074*
C50.3608 (6)0.4564 (7)0.4715 (8)0.056 (3)
H5A0.37380.45660.40150.084*
H5B0.37660.39720.48910.084*
H5C0.40350.49850.52900.084*
C60.3008 (6)0.5546 (7)0.8401 (6)0.049 (2)
H6A0.33730.50450.87220.073*
H6B0.27170.59450.89360.073*
H6C0.34780.58620.81950.073*
O70.1262 (3)0.3968 (4)0.4158 (4)0.0375 (14)
O80.0539 (3)0.4933 (4)0.2882 (4)0.0369 (14)
O90.1802 (4)0.5611 (4)0.5844 (5)0.0391 (14)
O100.0014 (4)0.6555 (4)0.4569 (4)0.0406 (15)
O110.0611 (4)0.6916 (4)0.6995 (5)0.0447 (15)
H110.07600.73830.74810.054*
O120.2113 (4)0.6128 (4)0.3535 (5)0.0461 (16)
H120.26230.64110.31740.055*
O130.1478 (4)0.5621 (4)0.3521 (5)0.0476 (16)
H130.18420.57730.31640.057*
B100.6254 (6)0.7575 (6)0.2496 (7)0.029 (2)
C110.6665 (6)0.6538 (6)0.1930 (8)0.044 (2)
F120.4992 (3)0.5922 (3)0.2695 (4)0.0524 (14)
C120.5963 (5)0.5769 (7)0.2022 (7)0.041 (2)
F130.5487 (4)0.4240 (4)0.1796 (5)0.0667 (16)
C130.6187 (6)0.4927 (7)0.1584 (8)0.046 (2)
F140.7441 (4)0.3892 (4)0.0406 (5)0.0769 (18)
C140.7202 (6)0.4741 (6)0.0949 (8)0.047 (2)
F150.8851 (4)0.5296 (4)0.0057 (5)0.0724 (18)
C150.7923 (7)0.5454 (8)0.0758 (8)0.056 (3)
F160.8383 (3)0.6956 (4)0.0962 (4)0.0532 (14)
C160.7630 (6)0.6307 (7)0.1220 (8)0.048 (2)
C210.5524 (5)0.7643 (5)0.1639 (7)0.034 (2)
F220.3850 (3)0.7414 (4)0.2903 (4)0.0539 (14)
C220.4445 (7)0.7549 (6)0.1844 (8)0.050 (3)
F230.2833 (3)0.7483 (4)0.1466 (5)0.0641 (16)
C230.3920 (6)0.7564 (7)0.1103 (10)0.060 (3)
C240.4376 (7)0.7656 (7)0.0060 (9)0.055 (3)
F240.3879 (5)0.7701 (4)0.0679 (5)0.0763 (18)
F250.5989 (4)0.7798 (4)0.1314 (4)0.0754 (18)
C250.5480 (8)0.7717 (7)0.0285 (8)0.060 (3)
F260.7038 (4)0.7759 (4)0.0148 (4)0.0570 (14)
C260.5977 (6)0.7712 (6)0.0498 (8)0.049 (2)
C310.5615 (6)0.7729 (6)0.3796 (7)0.044 (2)
F320.4895 (4)0.9015 (4)0.3638 (4)0.0545 (14)
C320.5005 (6)0.8429 (6)0.4285 (8)0.045 (2)
F330.3912 (5)0.9382 (4)0.5800 (5)0.0794 (19)
C330.4515 (7)0.8670 (7)0.5398 (9)0.061 (3)
F340.4135 (5)0.8359 (5)0.7215 (4)0.095 (2)
C340.4604 (9)0.8133 (8)0.6121 (9)0.068 (3)
F350.5342 (4)0.6922 (5)0.6367 (5)0.082 (2)
C350.5247 (7)0.7415 (8)0.5664 (7)0.055 (3)
F360.6279 (4)0.6488 (4)0.4219 (4)0.0587 (15)
C360.5707 (6)0.7224 (7)0.4551 (8)0.049 (2)
C410.7184 (6)0.8388 (7)0.2436 (7)0.043 (2)
F420.7987 (4)0.7506 (4)0.3270 (5)0.0590 (15)
C420.7970 (6)0.8263 (7)0.2928 (8)0.046 (2)
F430.9431 (4)0.8789 (5)0.3586 (5)0.0777 (19)
C430.8720 (6)0.8934 (8)0.3068 (8)0.056 (3)
F440.9501 (4)1.0379 (4)0.2838 (5)0.0816 (19)
C440.8765 (7)0.9704 (8)0.2734 (9)0.067 (3)
C450.8003 (7)0.9841 (6)0.2209 (8)0.049 (2)
F450.8000 (5)1.0628 (4)0.1894 (5)0.0822 (19)
F460.6533 (4)0.9399 (4)0.1677 (5)0.0607 (15)
C460.7212 (6)0.9205 (7)0.2146 (8)0.055 (3)
O900.1099 (6)0.8402 (6)0.8557 (8)0.088 (2)
H90A0.0880.8820.8200.105*
H90B0.17430.8440.8780.105*
Cl011.132 (3)0.927 (3)0.088 (4)0.116 (8)0.315 (5)
C1011.232 (2)0.9610 (17)0.150 (2)0.100 (5)*0.315 (5)
C1021.325 (2)0.996 (3)0.089 (2)0.100 (5)*0.315 (5)
H1021.33381.00140.01510.120*0.315 (5)
C1031.406 (2)1.024 (3)0.138 (3)0.100 (5)*0.315 (5)
H1031.46791.04740.09680.120*0.315 (5)
C1041.393 (2)1.016 (3)0.247 (3)0.100 (5)*0.315 (5)
H1041.44671.03440.28020.120*0.315 (5)
C1051.300 (3)0.981 (3)0.308 (3)0.100 (5)*0.315 (5)
H1051.29150.97550.38190.120*0.315 (5)
C1061.220 (2)0.953 (3)0.259 (3)0.100 (5)*0.315 (5)
H1061.15750.92960.30020.120*0.315 (5)
Cl111.111 (3)0.895 (3)0.076 (4)0.116 (8)0.315 (5)
C1111.207 (2)0.9370 (18)0.141 (3)0.100 (5)*0.315 (5)
C1121.303 (3)0.968 (3)0.080 (2)0.100 (5)*0.315 (5)
H1121.31510.96690.00430.120*0.315 (5)
C1131.380 (2)1.001 (3)0.133 (3)0.100 (5)*0.315 (5)
H1131.44331.02230.09180.120*0.315 (5)
C1141.361 (2)1.003 (3)0.246 (3)0.100 (5)*0.315 (5)
H1141.41241.02570.28130.120*0.315 (5)
C1151.266 (3)0.972 (3)0.307 (3)0.100 (5)*0.315 (5)
H1151.25320.97360.38320.120*0.315 (5)
C1161.189 (2)0.939 (3)0.255 (3)0.100 (5)*0.315 (5)
H1161.12500.91820.29570.120*0.315 (5)
Cl211.293 (6)1.026 (7)0.431 (4)0.145 (9)0.185 (5)
C1211.279 (4)1.000 (4)0.297 (3)0.085 (8)*0.185 (5)
C1221.187 (4)0.958 (4)0.278 (3)0.085 (8)*0.185 (5)
H1221.13390.94340.33720.102*0.185 (5)
C1231.176 (3)0.938 (4)0.170 (4)0.085 (8)*0.185 (5)
H1231.11520.91000.15790.102*0.185 (5)
C1241.256 (4)0.960 (4)0.082 (3)0.085 (8)*0.185 (5)
H1241.24890.94700.01000.102*0.185 (5)
C1251.348 (3)1.003 (4)0.101 (4)0.085 (8)*0.185 (5)
H1251.40121.01750.04140.102*0.185 (5)
C1261.359 (3)1.023 (4)0.208 (4)0.085 (8)*0.185 (5)
H1261.41991.05090.22080.102*0.185 (5)
Cl311.294 (6)1.013 (7)0.400 (4)0.145 (9)0.18
C1311.292 (4)0.994 (4)0.261 (3)0.085 (8)*0.185 (5)
C1321.200 (3)0.967 (4)0.233 (3)0.085 (8)*0.185 (5)
H1321.13950.95920.28910.102*0.185 (5)
C1331.199 (3)0.951 (4)0.123 (3)0.085 (8)*0.185 (5)
H1331.13700.93320.10410.102*0.185 (5)
C1341.289 (4)0.963 (4)0.040 (3)0.085 (8)*0.185 (5)
H1341.28830.95250.03460.102*0.185 (5)
C1351.381 (3)0.990 (4)0.067 (4)0.085 (8)*0.185 (5)
H1351.44200.99770.01170.102*0.185 (5)
C1361.383 (3)1.006 (4)0.178 (4)0.085 (8)*0.185 (5)
H1361.44451.02360.19670.102*0.185 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ga10.0226 (4)0.0617 (7)0.0356 (6)0.0006 (4)0.0117 (4)0.0080 (5)
Ga20.0209 (4)0.0522 (7)0.0435 (6)0.0053 (4)0.0099 (4)0.0082 (5)
Ga30.0206 (4)0.0570 (7)0.0387 (6)0.0011 (4)0.0097 (4)0.0132 (5)
Ga40.0214 (4)0.0534 (7)0.0410 (6)0.0029 (4)0.0083 (4)0.0060 (5)
Ga50.0153 (4)0.0602 (7)0.0409 (6)0.0028 (4)0.0110 (4)0.0106 (5)
Ga60.0180 (4)0.0610 (7)0.0344 (6)0.0003 (4)0.0064 (4)0.0069 (5)
C10.061 (6)0.085 (8)0.021 (5)0.002 (6)0.002 (4)0.005 (5)
C20.051 (6)0.047 (6)0.084 (8)0.007 (5)0.012 (6)0.010 (6)
C30.033 (5)0.053 (7)0.096 (8)0.001 (4)0.018 (5)0.015 (6)
C40.033 (5)0.060 (7)0.052 (6)0.016 (4)0.011 (4)0.000 (5)
C50.035 (5)0.078 (8)0.052 (6)0.016 (5)0.014 (4)0.014 (5)
C60.047 (5)0.079 (7)0.024 (5)0.007 (5)0.018 (4)0.003 (5)
O70.015 (2)0.057 (4)0.041 (3)0.008 (2)0.010 (2)0.011 (3)
O80.015 (2)0.064 (4)0.035 (3)0.005 (2)0.005 (2)0.016 (3)
O90.033 (3)0.046 (4)0.046 (4)0.002 (3)0.020 (3)0.014 (3)
O100.021 (3)0.050 (4)0.047 (4)0.001 (2)0.012 (3)0.002 (3)
O110.042 (3)0.043 (4)0.048 (4)0.004 (3)0.017 (3)0.002 (3)
O120.025 (3)0.054 (4)0.048 (4)0.006 (3)0.007 (3)0.011 (3)
O130.019 (3)0.069 (4)0.061 (4)0.005 (3)0.014 (3)0.021 (3)
B100.012 (4)0.045 (6)0.029 (5)0.001 (4)0.005 (4)0.005 (4)
C110.028 (4)0.049 (6)0.062 (6)0.004 (4)0.029 (4)0.005 (5)
F120.029 (2)0.071 (4)0.055 (3)0.010 (2)0.007 (2)0.018 (3)
C120.015 (4)0.068 (7)0.040 (5)0.000 (4)0.005 (4)0.013 (5)
F130.055 (3)0.061 (4)0.086 (4)0.001 (3)0.024 (3)0.014 (3)
C130.033 (5)0.051 (6)0.052 (6)0.011 (4)0.018 (4)0.005 (5)
F140.052 (3)0.081 (5)0.087 (4)0.005 (3)0.019 (3)0.011 (4)
C140.036 (5)0.038 (6)0.060 (6)0.003 (4)0.010 (4)0.004 (5)
F150.032 (3)0.106 (5)0.059 (4)0.009 (3)0.002 (3)0.011 (3)
C150.039 (5)0.084 (8)0.049 (6)0.014 (5)0.016 (5)0.009 (6)
F160.028 (2)0.072 (4)0.053 (3)0.005 (2)0.004 (2)0.012 (3)
C160.028 (5)0.063 (7)0.049 (6)0.002 (4)0.008 (4)0.008 (5)
C210.010 (3)0.030 (5)0.055 (6)0.000 (3)0.000 (4)0.005 (4)
F220.020 (2)0.085 (4)0.052 (3)0.008 (2)0.007 (2)0.013 (3)
C220.036 (5)0.046 (6)0.070 (7)0.002 (4)0.021 (5)0.005 (5)
F230.021 (2)0.093 (4)0.075 (4)0.005 (3)0.017 (2)0.009 (3)
C230.019 (4)0.076 (8)0.082 (8)0.004 (4)0.008 (5)0.016 (6)
C240.034 (5)0.059 (7)0.072 (8)0.007 (4)0.022 (5)0.003 (6)
F240.081 (4)0.105 (5)0.066 (4)0.002 (4)0.050 (3)0.027 (4)
F250.075 (4)0.111 (5)0.045 (4)0.000 (4)0.011 (3)0.033 (3)
C250.052 (6)0.082 (8)0.041 (6)0.009 (5)0.002 (5)0.011 (6)
F260.041 (3)0.076 (4)0.047 (3)0.001 (3)0.000 (2)0.014 (3)
C260.027 (4)0.057 (7)0.057 (6)0.003 (4)0.005 (4)0.010 (5)
C310.030 (4)0.057 (7)0.038 (5)0.007 (4)0.005 (4)0.005 (5)
F320.043 (3)0.061 (4)0.055 (3)0.000 (3)0.008 (2)0.009 (3)
C320.038 (5)0.052 (6)0.044 (6)0.008 (4)0.015 (5)0.007 (5)
F330.069 (4)0.082 (5)0.062 (4)0.003 (3)0.005 (3)0.018 (3)
C330.041 (5)0.050 (7)0.069 (8)0.012 (5)0.001 (5)0.013 (6)
F340.099 (5)0.138 (6)0.028 (3)0.010 (4)0.010 (3)0.007 (4)
C340.069 (7)0.078 (9)0.047 (7)0.049 (7)0.023 (6)0.005 (7)
F350.066 (4)0.129 (6)0.057 (4)0.024 (4)0.023 (3)0.035 (4)
C350.055 (6)0.077 (8)0.020 (5)0.016 (5)0.001 (5)0.009 (5)
F360.054 (3)0.077 (4)0.043 (3)0.010 (3)0.009 (3)0.019 (3)
C360.023 (4)0.063 (7)0.058 (7)0.013 (4)0.012 (4)0.013 (6)
C410.020 (4)0.073 (7)0.036 (5)0.007 (4)0.000 (4)0.026 (5)
F420.037 (3)0.066 (4)0.082 (4)0.006 (3)0.025 (3)0.023 (3)
C420.037 (5)0.052 (6)0.055 (6)0.007 (4)0.022 (4)0.015 (5)
F430.042 (3)0.125 (6)0.075 (4)0.001 (3)0.037 (3)0.010 (4)
C430.013 (4)0.083 (8)0.060 (7)0.005 (5)0.002 (4)0.001 (6)
F440.057 (4)0.069 (4)0.109 (5)0.022 (3)0.025 (3)0.005 (4)
C440.028 (5)0.067 (8)0.081 (8)0.010 (5)0.007 (5)0.002 (6)
C450.049 (6)0.037 (6)0.057 (6)0.004 (4)0.015 (5)0.004 (5)
F450.076 (4)0.063 (4)0.101 (5)0.024 (3)0.020 (4)0.023 (4)
F460.043 (3)0.066 (4)0.075 (4)0.007 (3)0.016 (3)0.022 (3)
C460.027 (5)0.071 (8)0.055 (6)0.011 (5)0.000 (4)0.005 (6)
O900.084 (6)0.072 (6)0.091 (7)0.005 (5)0.005 (5)0.011 (5)
Cl010.115 (14)0.13 (3)0.105 (10)0.019 (12)0.043 (7)0.002 (14)
Cl110.115 (14)0.13 (3)0.105 (10)0.019 (12)0.043 (7)0.002 (14)
Cl210.144 (11)0.13 (2)0.17 (2)0.030 (12)0.058 (19)0.02 (2)
Cl310.144 (11)0.13 (2)0.17 (2)0.030 (12)0.058 (19)0.02 (2)
Geometric parameters (Å, º) top
Ga1—O8i1.879 (6)C25—C261.358 (13)
Ga1—O7i1.898 (5)F26—C261.373 (9)
Ga1—O111.901 (6)C31—C321.351 (12)
Ga1—C11.915 (9)C31—C361.390 (12)
Ga2—O7i1.843 (6)F32—C321.380 (10)
Ga2—O101.898 (5)C32—C331.370 (13)
Ga2—C21.910 (9)F33—C331.350 (11)
Ga2—O121.950 (5)C33—C341.392 (15)
Ga3—O101.842 (5)F34—C341.342 (11)
Ga3—O81.868 (6)C34—C351.392 (15)
Ga3—C31.879 (10)F35—C351.324 (11)
Ga3—O131.929 (5)C35—C361.356 (12)
Ga4—O91.868 (6)F36—C361.355 (11)
Ga4—O101.884 (5)C41—C461.362 (13)
Ga4—O111.925 (5)C41—C421.430 (11)
Ga4—C41.945 (8)F42—C421.319 (10)
Ga5—O71.875 (5)C42—C431.381 (12)
Ga5—O91.881 (5)F43—C431.374 (11)
Ga5—C51.917 (8)C43—C441.318 (14)
Ga5—O131.920 (6)F44—C441.365 (11)
Ga6—O91.863 (5)C44—C451.436 (14)
Ga6—O8i1.876 (5)C45—F451.341 (10)
Ga6—O12i1.916 (6)C45—C461.372 (12)
Ga6—C61.934 (8)F46—C461.320 (11)
C1—H1A0.9600O90—H90A0.842
C1—H1B0.9600O90—H90B0.838
C1—H1C0.9600Cl01—C1011.7400
C2—H2A0.9600C101—C1021.3900
C2—H2B0.9600C101—C1061.3900
C2—H2C0.9600C102—C1031.3900
C3—H3A0.9600C102—H1020.9300
C3—H3B0.9600C103—C1041.3900
C3—H3C0.9600C103—H1030.9300
C4—H4A0.9600C104—C1051.3900
C4—H4B0.9600C104—H1040.9300
C4—H4C0.9600C105—C1061.3900
C5—H5A0.9600C105—H1050.9300
C5—H5B0.9600C106—H1060.9300
C5—H5C0.9600Cl11—C1111.7400
C6—H6A0.9600C111—C1121.3900
C6—H6B0.9600C111—C1161.3900
C6—H6C0.9600C112—C1131.3900
O7—Ga2i1.843 (6)C112—H1120.9300
O7—Ga1i1.898 (5)C113—C1141.3900
O8—Ga6i1.876 (5)C113—H1130.9300
O8—Ga1i1.879 (6)C114—C1151.3900
O11—H110.8400C114—H1140.9300
O12—Ga6i1.916 (6)C115—C1161.3900
O12—H120.8400C115—H1150.9300
O13—H130.8400C116—H1160.9300
B10—C311.613 (12)Cl21—C1211.7400
B10—C411.662 (12)C121—C1261.3900
B10—C111.677 (12)C121—C1221.3900
B10—C211.696 (11)C122—C1231.3900
C11—C161.389 (11)C122—H1220.9300
C11—C121.425 (12)C123—C1241.3900
F12—C121.358 (8)C123—H1230.9300
C12—C131.317 (12)C124—C1251.3900
F13—C131.348 (10)C124—H1240.9300
C13—C141.402 (12)C125—C1261.3900
F14—C141.357 (10)C125—H1250.9300
C14—C151.389 (13)C126—H1260.9300
F15—C151.326 (10)Cl31—C1311.7400
C15—C161.361 (13)C131—C1361.3900
F16—C161.357 (10)C131—C1321.3900
C21—C221.403 (11)C132—C1331.3900
C21—C261.427 (12)C132—H1320.9300
F22—C221.401 (10)C133—C1341.3900
C22—C231.343 (13)C133—H1330.9300
F23—C231.406 (9)C134—C1351.3900
C23—C241.324 (13)C134—H1340.9300
C24—F241.324 (10)C135—C1361.3900
C24—C251.428 (12)C135—H1350.9300
F25—C251.317 (10)C136—H1360.9300
O8i—Ga1—O7i102.2 (2)F22—C22—C21118.2 (8)
O8i—Ga1—O1198.5 (2)C24—C23—C22123.1 (8)
O7i—Ga1—O1197.5 (2)C24—C23—F23119.1 (9)
O8i—Ga1—C1122.3 (3)C22—C23—F23117.8 (9)
O7i—Ga1—C1118.9 (3)F24—C24—C23124.5 (9)
O11—Ga1—C1113.1 (4)F24—C24—C25118.0 (10)
O7i—Ga2—O10104.3 (2)C23—C24—C25117.5 (9)
O7i—Ga2—C2119.2 (4)F25—C25—C26121.7 (9)
O10—Ga2—C2121.4 (4)F25—C25—C24121.0 (9)
O7i—Ga2—O1297.8 (2)C26—C25—C24117.2 (9)
O10—Ga2—O1296.9 (2)C25—C26—F26116.4 (8)
C2—Ga2—O12112.7 (3)C25—C26—C21127.5 (8)
O10—Ga3—O8104.1 (2)F26—C26—C21116.0 (8)
O10—Ga3—C3119.8 (4)C32—C31—C36112.8 (9)
O8—Ga3—C3117.9 (3)C32—C31—B10122.4 (9)
O10—Ga3—O1396.1 (2)C36—C31—B10124.5 (8)
O8—Ga3—O1397.8 (2)C31—C32—C33126.9 (10)
C3—Ga3—O13117.0 (3)C31—C32—F32118.7 (8)
O9—Ga4—O10101.8 (2)C33—C32—F32114.3 (9)
O9—Ga4—O1197.7 (2)F33—C33—C32122.1 (11)
O10—Ga4—O1199.6 (2)F33—C33—C34119.3 (10)
O9—Ga4—C4119.8 (3)C32—C33—C34118.4 (10)
O10—Ga4—C4121.7 (3)F34—C34—C35123.6 (11)
O11—Ga4—C4112.0 (3)F34—C34—C33119.4 (12)
O7—Ga5—O9103.2 (2)C35—C34—C33116.9 (10)
O7—Ga5—C5117.0 (3)F35—C35—C36122.9 (11)
O9—Ga5—C5120.1 (3)F35—C35—C34116.2 (9)
O7—Ga5—O1398.1 (2)C36—C35—C34120.9 (11)
O9—Ga5—O1398.0 (2)F36—C36—C35114.4 (10)
C5—Ga5—O13116.7 (3)F36—C36—C31121.6 (8)
O9—Ga6—O8i104.4 (2)C35—C36—C31124.0 (10)
O9—Ga6—O12i98.9 (3)C46—C41—C42116.1 (8)
O8i—Ga6—O12i97.2 (2)C46—C41—B10128.7 (8)
O9—Ga6—C6115.5 (3)C42—C41—B10114.3 (8)
O8i—Ga6—C6123.1 (3)F42—C42—C43118.5 (8)
O12i—Ga6—C6113.6 (3)F42—C42—C41120.5 (8)
Ga1—C1—H1A109.5C43—C42—C41120.9 (9)
Ga1—C1—H1B109.5C44—C43—F43119.5 (9)
H1A—C1—H1B109.5C44—C43—C42122.2 (10)
Ga1—C1—H1C109.5F43—C43—C42118.3 (10)
H1A—C1—H1C109.5C43—C44—F44124.2 (11)
H1B—C1—H1C109.5C43—C44—C45118.3 (9)
Ga2—C2—H2A109.5F44—C44—C45117.5 (10)
Ga2—C2—H2B109.5F45—C45—C46120.0 (9)
H2A—C2—H2B109.5F45—C45—C44120.1 (8)
Ga2—C2—H2C109.5C46—C45—C44119.5 (10)
H2A—C2—H2C109.5F46—C46—C41121.8 (8)
H2B—C2—H2C109.5F46—C46—C45115.4 (10)
Ga3—C3—H3A109.5C41—C46—C45122.5 (10)
Ga3—C3—H3B109.5H90A—O90—H90B105.2
H3A—C3—H3B109.5C102—C101—C106120.0
Ga3—C3—H3C109.5C102—C101—Cl01120.0
H3A—C3—H3C109.5C106—C101—Cl01120.0
H3B—C3—H3C109.5C101—C102—C103120.0
Ga4—C4—H4A109.5C101—C102—H102120.0
Ga4—C4—H4B109.5C103—C102—H102120.0
H4A—C4—H4B109.5C104—C103—C102120.0
Ga4—C4—H4C109.5C104—C103—H103120.0
H4A—C4—H4C109.5C102—C103—H103120.0
H4B—C4—H4C109.5C105—C104—C103120.0
Ga5—C5—H5A109.5C105—C104—H104120.0
Ga5—C5—H5B109.5C103—C104—H104120.0
H5A—C5—H5B109.5C106—C105—C104120.0
Ga5—C5—H5C109.5C106—C105—H105120.0
H5A—C5—H5C109.5C104—C105—H105120.0
H5B—C5—H5C109.5C105—C106—C101120.0
Ga6—C6—H6A109.5C105—C106—H106120.0
Ga6—C6—H6B109.5C101—C106—H106120.0
H6A—C6—H6B109.5C112—C111—C116120.0
Ga6—C6—H6C109.5C112—C111—Cl11120.0
H6A—C6—H6C109.5C116—C111—Cl11120.0
H6B—C6—H6C109.5C111—C112—C113120.0
Ga2i—O7—Ga5120.9 (3)C111—C112—H112120.0
Ga2i—O7—Ga1i119.4 (3)C113—C112—H112120.0
Ga5—O7—Ga1i119.7 (3)C114—C113—C112120.0
Ga3—O8—Ga6i120.1 (3)C114—C113—H113120.0
Ga3—O8—Ga1i120.7 (2)C112—C113—H113120.0
Ga6i—O8—Ga1i118.9 (3)C113—C114—C115120.0
Ga6—O9—Ga4120.0 (3)C113—C114—H114120.0
Ga6—O9—Ga5119.4 (3)C115—C114—H114120.0
Ga4—O9—Ga5120.5 (3)C116—C115—C114120.0
Ga3—O10—Ga4123.5 (3)C116—C115—H115120.0
Ga3—O10—Ga2119.8 (3)C114—C115—H115120.0
Ga4—O10—Ga2116.6 (3)C111—C116—C115120.0
Ga1—O11—Ga4129.0 (3)C111—C116—H116120.0
Ga1—O11—H11115.5C115—C116—H116120.0
Ga4—O11—H11115.5C126—C121—C122120.0
Ga6i—O12—Ga2127.7 (3)C126—C121—Cl21120.0
Ga6i—O12—H12116.2C122—C121—Cl21120.0
Ga2—O12—H12116.2C123—C122—C121120.0
Ga5—O13—Ga3128.5 (3)C123—C122—H122120.0
Ga5—O13—H13115.8C121—C122—H122120.0
Ga3—O13—H13115.8C124—C123—C122120.0
C31—B10—C41103.7 (6)C124—C123—H123120.0
C31—B10—C11115.9 (7)C122—C123—H123120.0
C41—B10—C11114.9 (6)C123—C124—C125120.0
C31—B10—C21113.3 (6)C123—C124—H124120.0
C41—B10—C21110.9 (7)C125—C124—H124120.0
C11—B10—C2198.3 (6)C126—C125—C124120.0
C16—C11—C12111.4 (8)C126—C125—H125120.0
C16—C11—B10127.3 (8)C124—C125—H125120.0
C12—C11—B10120.8 (7)C121—C126—C125120.0
C13—C12—F12117.4 (8)C121—C126—H126120.0
C13—C12—C11126.3 (8)C125—C126—H126120.0
F12—C12—C11116.1 (8)C136—C131—C132120.0
C12—C13—F13121.7 (8)C136—C131—Cl31120.0
C12—C13—C14118.9 (8)C132—C131—Cl31120.0
F13—C13—C14119.3 (9)C133—C132—C131120.0
F14—C14—C15120.2 (8)C133—C132—H132120.0
F14—C14—C13120.5 (8)C131—C132—H132120.0
C15—C14—C13118.8 (9)C132—C133—C134120.0
F15—C15—C16121.3 (9)C132—C133—H133120.0
F15—C15—C14119.5 (9)C134—C133—H133120.0
C16—C15—C14119.0 (8)C135—C134—C133120.0
F16—C16—C15114.4 (8)C135—C134—H134120.0
F16—C16—C11120.3 (9)C133—C134—H134120.0
C15—C16—C11125.3 (9)C134—C135—C136120.0
C22—C21—C26108.9 (8)C134—C135—H135120.0
C22—C21—B10128.9 (8)C136—C135—H135120.0
C26—C21—B10121.9 (6)C131—C136—C135120.0
C23—C22—F22116.1 (8)C131—C136—H136120.0
C23—C22—C21125.7 (9)C135—C136—H136120.0
O9—Ga5—O7—Ga2i62.6 (3)F23—C23—C24—F241.9 (16)
C5—Ga5—O7—Ga2i71.6 (4)C22—C23—C24—C251.6 (16)
O13—Ga5—O7—Ga2i162.9 (3)F23—C23—C24—C25178.7 (9)
O9—Ga5—O7—Ga1i115.0 (3)F24—C24—C25—F251.4 (15)
C5—Ga5—O7—Ga1i110.8 (4)C23—C24—C25—F25179.1 (10)
O13—Ga5—O7—Ga1i14.8 (3)F24—C24—C25—C26177.0 (9)
O10—Ga3—O8—Ga6i62.3 (3)C23—C24—C25—C262.5 (15)
C3—Ga3—O8—Ga6i73.2 (5)F25—C25—C26—F262.5 (15)
O13—Ga3—O8—Ga6i160.6 (3)C24—C25—C26—F26179.1 (8)
O10—Ga3—O8—Ga1i111.6 (3)F25—C25—C26—C21179.1 (9)
C3—Ga3—O8—Ga1i113.0 (4)C24—C25—C26—C210.7 (16)
O13—Ga3—O8—Ga1i13.3 (3)C22—C21—C26—C251.8 (14)
O8i—Ga6—O9—Ga462.0 (3)B10—C21—C26—C25175.8 (9)
O12i—Ga6—O9—Ga4161.9 (3)C22—C21—C26—F26176.6 (7)
C6—Ga6—O9—Ga476.5 (4)B10—C21—C26—F262.6 (12)
O8i—Ga6—O9—Ga5112.7 (3)C41—B10—C31—C3271.4 (10)
O12i—Ga6—O9—Ga512.8 (3)C11—B10—C31—C32161.6 (7)
C6—Ga6—O9—Ga5108.9 (4)C21—B10—C31—C3249.0 (11)
O10—Ga4—O9—Ga6114.9 (3)C41—B10—C31—C36101.8 (9)
O11—Ga4—O9—Ga613.4 (3)C11—B10—C31—C3625.2 (11)
C4—Ga4—O9—Ga6107.5 (4)C21—B10—C31—C36137.8 (8)
O10—Ga4—O9—Ga559.6 (3)C36—C31—C32—C331.0 (13)
O11—Ga4—O9—Ga5161.2 (3)B10—C31—C32—C33173.0 (8)
C4—Ga4—O9—Ga577.9 (4)C36—C31—C32—F32176.4 (7)
O7—Ga5—O9—Ga661.5 (3)B10—C31—C32—F322.5 (12)
C5—Ga5—O9—Ga671.0 (5)C31—C32—C33—F33179.4 (8)
O13—Ga5—O9—Ga6161.8 (3)F32—C32—C33—F334.9 (12)
O7—Ga5—O9—Ga4113.2 (3)C31—C32—C33—C342.7 (14)
C5—Ga5—O9—Ga4114.4 (4)F32—C32—C33—C34178.4 (8)
O13—Ga5—O9—Ga412.8 (3)F33—C33—C34—F343.5 (13)
O8—Ga3—O10—Ga4113.3 (3)C32—C33—C34—F34179.7 (8)
C3—Ga3—O10—Ga4112.2 (4)F33—C33—C34—C35179.1 (8)
O13—Ga3—O10—Ga413.7 (4)C32—C33—C34—C354.1 (13)
O8—Ga3—O10—Ga262.1 (4)F34—C34—C35—F353.1 (14)
C3—Ga3—O10—Ga272.3 (5)C33—C34—C35—F35178.6 (8)
O13—Ga3—O10—Ga2161.7 (3)F34—C34—C35—C36179.5 (8)
O9—Ga4—O10—Ga361.8 (4)C33—C34—C35—C364.1 (14)
O11—Ga4—O10—Ga3161.9 (3)F35—C35—C36—F360.5 (13)
C4—Ga4—O10—Ga374.8 (5)C34—C35—C36—F36177.7 (8)
O9—Ga4—O10—Ga2113.8 (3)F35—C35—C36—C31179.7 (8)
O11—Ga4—O10—Ga213.7 (4)C34—C35—C36—C312.5 (14)
C4—Ga4—O10—Ga2109.7 (4)C32—C31—C36—F36179.4 (7)
O7i—Ga2—O10—Ga3112.4 (3)B10—C31—C36—F366.8 (13)
C2—Ga2—O10—Ga3109.5 (5)C32—C31—C36—C350.8 (13)
O12—Ga2—O10—Ga312.5 (4)B10—C31—C36—C35173.0 (8)
O7i—Ga2—O10—Ga463.3 (3)C31—B10—C41—C4697.3 (10)
C2—Ga2—O10—Ga474.8 (5)C11—B10—C41—C46135.1 (9)
O12—Ga2—O10—Ga4163.2 (3)C21—B10—C41—C4624.7 (12)
O8i—Ga1—O11—Ga452.4 (4)C31—B10—C41—C4271.5 (9)
O7i—Ga1—O11—Ga451.2 (4)C11—B10—C41—C4256.1 (10)
C1—Ga1—O11—Ga4177.0 (4)C21—B10—C41—C42166.5 (7)
O9—Ga4—O11—Ga152.1 (4)C46—C41—C42—F42177.8 (8)
O10—Ga4—O11—Ga151.3 (4)B10—C41—C42—F427.5 (12)
C4—Ga4—O11—Ga1178.7 (4)C46—C41—C42—C431.5 (13)
O7i—Ga2—O12—Ga6i51.2 (4)B10—C41—C42—C43171.8 (8)
O10—Ga2—O12—Ga6i54.3 (4)F42—C42—C43—C44179.0 (9)
C2—Ga2—O12—Ga6i177.4 (5)C41—C42—C43—C441.7 (15)
O7—Ga5—O13—Ga351.4 (4)F42—C42—C43—F431.8 (13)
O9—Ga5—O13—Ga353.3 (4)C41—C42—C43—F43177.5 (8)
C5—Ga5—O13—Ga3177.2 (4)F43—C43—C44—F441.9 (15)
O10—Ga3—O13—Ga552.7 (4)C42—C43—C44—F44178.9 (9)
O8—Ga3—O13—Ga552.4 (4)F43—C43—C44—C45179.1 (8)
C3—Ga3—O13—Ga5179.3 (5)C42—C43—C44—C450.0 (15)
C31—B10—C11—C16136.6 (9)C43—C44—C45—F45177.6 (9)
C41—B10—C11—C1615.4 (12)F44—C44—C45—F453.4 (13)
C21—B10—C11—C16102.4 (9)C43—C44—C45—C464.9 (14)
C31—B10—C11—C1252.5 (10)F44—C44—C45—C46176.1 (8)
C41—B10—C11—C12173.7 (7)C42—C41—C46—F46179.5 (8)
C21—B10—C11—C1268.5 (9)B10—C41—C46—F4611.9 (14)
C16—C11—C12—C135.4 (14)C42—C41—C46—C456.5 (13)
B10—C11—C12—C13177.6 (8)B10—C41—C46—C45175.2 (8)
C16—C11—C12—F12179.6 (7)F45—C45—C46—F465.5 (13)
B10—C11—C12—F127.4 (12)C44—C45—C46—F46178.2 (8)
F12—C12—C13—F130.6 (13)F45—C45—C46—C41178.8 (8)
C11—C12—C13—F13174.4 (8)C44—C45—C46—C418.4 (14)
F12—C12—C13—C14175.6 (8)C106—C101—C102—C1030.0
C11—C12—C13—C140.7 (15)Cl01—C101—C102—C103180.0
C12—C13—C14—F14174.4 (9)C101—C102—C103—C1040.0
F13—C13—C14—F1410.4 (14)C102—C103—C104—C1050.0
C12—C13—C14—C153.3 (14)C103—C104—C105—C1060.0
F13—C13—C14—C15178.5 (8)C104—C105—C106—C1010.0
F14—C14—C15—F151.2 (14)C102—C101—C106—C1050.0
C13—C14—C15—F15172.4 (8)Cl01—C101—C106—C105180.0
F14—C14—C15—C16173.1 (9)C116—C111—C112—C1130.0
C13—C14—C15—C162.0 (15)Cl11—C111—C112—C113180.0
F15—C15—C16—F164.3 (13)C111—C112—C113—C1140.0
C14—C15—C16—F16178.6 (8)C112—C113—C114—C1150.0
F15—C15—C16—C11177.7 (8)C113—C114—C115—C1160.0
C14—C15—C16—C113.4 (15)C112—C111—C116—C1150.0
C12—C11—C16—F16175.4 (8)Cl11—C111—C116—C115180.0
B10—C11—C16—F163.8 (14)C114—C115—C116—C1110.0
C12—C11—C16—C156.7 (14)C126—C121—C122—C1230.0
B10—C11—C16—C15178.3 (9)Cl21—C121—C122—C123180.0
C31—B10—C21—C2220.5 (12)C121—C122—C123—C1240.0
C41—B10—C21—C22136.7 (9)C122—C123—C124—C1250.0
C11—B10—C21—C22102.5 (9)C123—C124—C125—C1260.0
C31—B10—C21—C26166.8 (8)C122—C121—C126—C1250.0
C41—B10—C21—C2650.6 (10)Cl21—C121—C126—C125180.0
C11—B10—C21—C2670.2 (9)C124—C125—C126—C1210.0
C26—C21—C22—C232.9 (13)C136—C131—C132—C1330.0
B10—C21—C22—C23176.3 (9)Cl31—C131—C132—C133180.0
C26—C21—C22—F22176.2 (7)C131—C132—C133—C1340.0
B10—C21—C22—F222.8 (13)C132—C133—C134—C1350.0
F22—C22—C23—C24177.7 (9)C133—C134—C135—C1360.0
C21—C22—C23—C241.4 (17)C132—C131—C136—C1350.0
F22—C22—C23—F232.5 (13)Cl31—C131—C136—C135180.0
C21—C22—C23—F23178.3 (8)C134—C135—C136—C1310.0
C22—C23—C24—F24177.9 (9)
Symmetry code: (i) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O11—H11···O900.841.852.686 (10)179
O12—H12···F220.842.132.924 (7)157
O90—H90A···F44ii0.842.333.090 (10)150
O90—H90B···F26iii0.842.362.955 (10)129
Symmetry codes: (ii) x1, y+2, z+1; (iii) x+1, y, z+1.

Experimental details

Crystal data
Chemical formula[Ga12C12H42O14](C24F20B)2·2C6H5Cl·2H2O
Mr2866.32
Crystal system, space groupTriclinic, P1
Temperature (K)210
a, b, c (Å)13.532 (3), 15.223 (5), 12.755 (3)
α, β, γ (°)101.98 (2), 106.91 (2), 83.71 (2)
V3)2455.7 (11)
Z1
Radiation typeMo Kα
µ (mm1)3.42
Crystal size (mm)0.34 × 0.28 × 0.18
Data collection
DiffractometerEnraf-Nonius CAD-4
diffractometer
Absorption correctionψ scans
(MolEN; Fair, 1990)
Tmin, Tmax0.329, 0.540
No. of measured, independent and
observed [I > 2σ(I)] reflections
10851, 8067, 4561
Rint0.073
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.056, 0.122, 1.11
No. of reflections8067
No. of parameters620
No. of restraints3
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.55, 0.76

Computer programs: CAD-4 Operations Manual (Enraf-Nonius, 1977), CAD-4 Operations Manual, MolEN (Fair, 1990), SHELXTL (Sheldrick, 1995), SHELXL97 (Sheldrick, 1997), SHELXTL.

Selected geometric parameters (Å, º) top
Ga1—O8i1.879 (6)Ga4—O91.868 (6)
Ga1—O7i1.898 (5)Ga4—O101.884 (5)
Ga1—O111.901 (6)Ga4—O111.925 (5)
Ga1—C11.915 (9)Ga4—C41.945 (8)
Ga2—O7i1.843 (6)Ga5—O71.875 (5)
Ga2—O101.898 (5)Ga5—O91.881 (5)
Ga2—C21.910 (9)Ga5—C51.917 (8)
Ga2—O121.950 (5)Ga5—O131.920 (6)
Ga3—O101.842 (5)Ga6—O91.863 (5)
Ga3—O81.868 (6)Ga6—O8i1.876 (5)
Ga3—C31.879 (10)Ga6—O12i1.916 (6)
Ga3—O131.929 (5)Ga6—C61.934 (8)
O8i—Ga1—O7i102.2 (2)O9—Ga5—C5120.1 (3)
O8i—Ga1—O1198.5 (2)O7—Ga5—O1398.1 (2)
O7i—Ga1—O1197.5 (2)O9—Ga5—O1398.0 (2)
O8i—Ga1—C1122.3 (3)C5—Ga5—O13116.7 (3)
O7i—Ga1—C1118.9 (3)O9—Ga6—O8i104.4 (2)
O11—Ga1—C1113.1 (4)O9—Ga6—O12i98.9 (3)
O7i—Ga2—O10104.3 (2)O8i—Ga6—O12i97.2 (2)
O7i—Ga2—C2119.2 (4)O9—Ga6—C6115.5 (3)
O10—Ga2—C2121.4 (4)O8i—Ga6—C6123.1 (3)
O7i—Ga2—O1297.8 (2)O12i—Ga6—C6113.6 (3)
O10—Ga2—O1296.9 (2)Ga2i—O7—Ga5120.9 (3)
C2—Ga2—O12112.7 (3)Ga2i—O7—Ga1i119.4 (3)
O10—Ga3—O8104.1 (2)Ga5—O7—Ga1i119.7 (3)
O10—Ga3—C3119.8 (4)Ga3—O8—Ga6i120.1 (3)
O8—Ga3—C3117.9 (3)Ga3—O8—Ga1i120.7 (2)
O10—Ga3—O1396.1 (2)Ga6i—O8—Ga1i118.9 (3)
O8—Ga3—O1397.8 (2)Ga6—O9—Ga4120.0 (3)
C3—Ga3—O13117.0 (3)Ga6—O9—Ga5119.4 (3)
O9—Ga4—O10101.8 (2)Ga4—O9—Ga5120.5 (3)
O9—Ga4—O1197.7 (2)Ga3—O10—Ga4123.5 (3)
O10—Ga4—O1199.6 (2)Ga3—O10—Ga2119.8 (3)
O9—Ga4—C4119.8 (3)Ga4—O10—Ga2116.6 (3)
O10—Ga4—C4121.7 (3)Ga1—O11—Ga4129.0 (3)
O11—Ga4—C4112.0 (3)Ga6i—O12—Ga2127.7 (3)
O7—Ga5—O9103.2 (2)Ga5—O13—Ga3128.5 (3)
O7—Ga5—C5117.0 (3)
Symmetry code: (i) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O11—H11···O900.841.852.686 (10)179
O12—H12···F220.842.132.924 (7)157
O90—H90A···F44ii0.842.333.090 (10)150
O90—H90B···F26iii0.842.362.955 (10)129
Symmetry codes: (ii) x1, y+2, z+1; (iii) x+1, y, z+1.
 

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