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In the title compound, [Ga(C12H18N2O2)Cl], the Ga atom is coordinated to a Cl atom and the two imine N and two enolate O atoms of the Schiff base ligand. The literature reveals few examples of a five-coordinate GaO2N2Cl environment, and only two where both the N and the O atoms are contained within the same ligand. This configuration has the effect of constraining the complex into a square-pyramidal geometry with less distortion than if formed by two or more ligands. The Ga-N and Ga-O distances are within the ranges expected for Ga-Schiff base derivatives. This compound is also the first group 13 complex containing the N,N'-ethyl­ene­bis­(acetyl­acetoneimine) (acacen) ligand.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270105013594/hj1048sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270105013594/hj1048Isup2.hkl
Contains datablock I

CCDC reference: 250665

Comment top

There has been recent interest in the design of methodology en route toward metal oxynitrides, possessing intermediate properties between oxide and nitride phases (Kim et al., 2000; Pan et al., 1985; Erlat et al., 2004). Novel materials composed of group 13 oxynitrides have recently been used as supports for catalytic applications (Delsarte et al., 2003; Centeno et al., 2000) and high-temperature ceramics (Cao & Metselaar, 1991; Hwang & Chen, 1994; Ryabora & Savitskaya, 1968). The sputter deposition of aluminium oxynitride films onto polymer matrices has recently been found to impart superior water vapor permeation resistance (Delsarte et al., 2003).

We are focused on the design of single-source precursors for oxynitride films and nanostructural materials. Such suitable compounds must contain both M—O and M—N units; for certain applications, the backbone of the ligand should also contain small amounts of carbon. For oxide thin films, metal B-diketonate complexes have been widely used because of their low cost, stability, high volatility, low toxicity, and lack of M—C bonds (Barron, 1996). Furthermore, the volatility of these complexes has been found to change dramatically upon substitution of fluorine for hydrogen groups, allowing for fine tuning of the deposition conditions (Fahlman & Barron, 2000).

Compounds that contain the Schiff base ligand N,N'-ethylenebis(acetylacetoneimine) (acacen) may represent a suitable class of materials for oxynitride-based materials, because of the relatively low carbon content and the presence of direct M—O and M—N bonds. This ligand system has been well studied, as numerous transition metal (Baker et al., 1970; Larkworthy et al., 1984; Gambarotta et al., 1985) and rare earth complexes (Cai et al., 2001; Junk & Smith, 2003) have been isolated. Metal–acacen complexes are comparable to those containing the salen family of ligands, which are widely employed for catalytic applications (Atwood & Harvey, 2001). We have now synthesized the title complex, (I), and it represents the first use of this ligand on a group 13 metal, and only the second on a main-group metal (Ewings et al., 1976). The most common method used to synthesize metal–acacen complexes consists of exothermic reactions between the neutral acacenH2 moiety and a metal alkyl (Baker et al., 1970; Larkworthy et al., 1984; Gambarotta et al., 1985; Cai et al., 2001; Junk & Smith, 2003). However, this route was not successful with regard to the group 13 analogs, and we instead used the reaction of an Na2(acacen) salt with the correponding metal chloride.

A number of points regarding the structure and bonding in (I) (Fig. 1) are relevant. The compound contains a five-coordinate Ga atom in a distorted square-pyramidal geometry, with the ligand occupying the basal plane at a Ga—N2O2 plane distance of 0.47 Å. The Cl atom occupies the apical site at a distance of 2.2237 (4) Å. The average Ga—O and Ga—N bond distances are 1.91 and 2.00 Å, respectively, and are comparable to those of analogous salen derivatives (Atwood & Harvey). When comparing this structure with other complexes with GaN2O2Cl coordination environments, it is apparent that having a single N2O2 four-coordinate ligand lessens the level of distortion from the ideal square pyramidal geometry. Indeed, in systems where the ligands are allowed to rotate more freely, the geometry is much more distorted. Furthermore, when comparing this group 13 metal–acacen complex to one of the numerous five-coordinate transition metal complexes, the geometries are very similar (Clark et al., 1969; Sato et al., 1981). Thus far, our attempts to grow single crystals of the aluminium analogue have not been successful.

Experimental top

For the preparation of the title compound, which was carried out under an inert atmosphere, Na2(acacen) (2.149 g, 8.01 mmol), prepared from the reaction of N,N'-ethylenebis(acetylacetoneimine) and NaH, was added slowly via a solid addition funnel to a stirring solution of GaCl3 (1.49 g, 8.00 mmol) in benzene. The reaction was then stirred overnight at room temperature. The yellow solution was filtered and the precipitant was washed with benzene to extract additional product. The solution was dried in vacuo and recrystallized via sublimation to yield yellow crystals suitable for X-ray crystallographic analysis.

Refinement top

A measure of disorder was observed for atoms C11 and C12 and their adjacent positions, with occupancies of approximately 60:40%. H atoms on disordered C atoms were placed in calculated positions and treated using a riding model (C—H = 0.97 Å). All other H atoms were freely refined [C—H = 0.88 (3)–1.05 (3) Å].

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); 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 molecular structure of (I), with the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level and H atoms are shown as small spheres of arbitrary radii. Atoms of the lower fraction of the disordered part of the molecule have been omitted for clarity.
[N,N'-Ethylenediiminobis(acetylacetonato)]chlorogallium(III) top
Crystal data top
[Ga(C12H18N2O2)Cl]F(000) = 672
Mr = 327.45Dx = 1.584 Mg m3
Monoclinic, P21/nMelting point: 204 K
Hall symbol: -P2ynMo Kα radiation, λ = 0.71073 Å
a = 7.2163 (6) ÅCell parameters from 2980 reflections
b = 24.102 (2) Åθ = 1.7–28.3°
c = 8.0669 (7) ŵ = 2.19 mm1
β = 101.776 (1)°T = 163 K
V = 1373.5 (2) Å3Plate, light yellow
Z = 40.33 × 0.20 × 0.12 mm
Data collection top
Bruker SMART CCD
diffractometer
3298 independent reflections
Radiation source: fine-focus sealed tube2992 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
ϕ and ω scansθmax = 28.3°, θmin = 1.7°
Absorption correction: empirical (using intensity measurements)
(SADABS; Bruker, 1998)
h = 99
Tmin = 0.531, Tmax = 0.779k = 3131
14190 measured reflectionsl = 1010
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)] = 0.020Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.051H atoms treated by a mixture of independent and constrained refinement
S = 1.08 w = 1/[σ2(Fo2) + (0.0217P)2 + 0.5951P]
where P = (Fo2 + 2Fc2)/3
3298 reflections(Δ/σ)max = 0.001
239 parametersΔρmax = 0.32 e Å3
0 restraintsΔρmin = 0.25 e Å3
Crystal data top
[Ga(C12H18N2O2)Cl]V = 1373.5 (2) Å3
Mr = 327.45Z = 4
Monoclinic, P21/nMo Kα radiation
a = 7.2163 (6) ŵ = 2.19 mm1
b = 24.102 (2) ÅT = 163 K
c = 8.0669 (7) Å0.33 × 0.20 × 0.12 mm
β = 101.776 (1)°
Data collection top
Bruker SMART CCD
diffractometer
3298 independent reflections
Absorption correction: empirical (using intensity measurements)
(SADABS; Bruker, 1998)
2992 reflections with I > 2σ(I)
Tmin = 0.531, Tmax = 0.779Rint = 0.024
14190 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0200 restraints
wR(F2) = 0.051H atoms treated by a mixture of independent and constrained refinement
S = 1.08Δρmax = 0.32 e Å3
3298 reflectionsΔρmin = 0.25 e Å3
239 parameters
Special details top

Experimental. Elemental Analyses: Anal·(Chemisar Laboratories, Inc, Guelph, Ontario, Canada). Calc. (found) for C12H18ClGaN2O2: C, 44.01 (44.13); H, 5.54 (5.61)%. 1H(300 MHz, 298 K, C6D6): 1.30 [s, 6H, CH3], 1.89 [s, 6H, CH3], 2.48 [q, JCH = 7 Hz, 2H, = CH2], 3.02 [q, JCH = 7 Hz, 2H, CH2], 4.82 [s, 2H, CH] 13C(75 MHz, 298 K, = C6D6): 27.33, 31.70, 50.00, 103.08, 177.73, 185.43. MS m/z 328 (M + H)+

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*/UeqOcc. (<1)
Ga10.42884 (2)0.126226 (6)0.688556 (18)0.01465 (5)
Cl10.24796 (5)0.062662 (14)0.53377 (4)0.02138 (8)
O10.32351 (15)0.19524 (4)0.59564 (13)0.0209 (2)
O20.30059 (16)0.14324 (5)0.86696 (13)0.0238 (2)
N10.64611 (18)0.13472 (5)0.57333 (17)0.0235 (3)
N20.61844 (18)0.08040 (5)0.84724 (16)0.0215 (3)
C10.2578 (3)0.27584 (7)0.4278 (2)0.0308 (4)
C20.3839 (2)0.22712 (6)0.48766 (18)0.0215 (3)
C30.5470 (2)0.21946 (7)0.4289 (2)0.0258 (3)
C40.6761 (2)0.17499 (7)0.47261 (18)0.0229 (3)
C50.8530 (3)0.17561 (10)0.4006 (3)0.0418 (5)
C60.1966 (3)0.14418 (9)1.1242 (2)0.0310 (4)
C70.3351 (2)0.12432 (6)1.02110 (18)0.0214 (3)
C80.4815 (2)0.08999 (7)1.09081 (19)0.0240 (3)
C90.6210 (2)0.06896 (6)1.00652 (18)0.0206 (3)
C100.7733 (3)0.03274 (8)1.1081 (2)0.0316 (4)
C110.8083 (6)0.0970 (2)0.6444 (6)0.0271 (10)0.604 (12)
H11A0.91070.11830.71180.033*0.604 (12)
H11B0.85520.07950.55270.033*0.604 (12)
C120.7417 (13)0.0530 (3)0.7538 (10)0.0273 (12)0.587 (19)
H12A0.67410.02370.68360.033*0.587 (19)
H12B0.84880.03670.83060.033*0.587 (19)
C11B0.7474 (10)0.0809 (2)0.5804 (9)0.0211 (15)0.396 (12)
H11C0.86360.08470.53850.025*0.396 (12)
H11D0.66850.05280.51470.025*0.396 (12)
C12B0.7890 (15)0.0666 (5)0.7690 (14)0.0237 (16)0.413 (19)
H12C0.89850.08730.82660.028*0.413 (19)
H12D0.81810.02730.78350.028*0.413 (19)
H1A0.223 (4)0.2943 (10)0.519 (3)0.058 (7)*
H1B0.149 (4)0.2645 (11)0.361 (3)0.061 (7)*
H1C0.313 (4)0.3024 (11)0.368 (3)0.059 (7)*
H30.576 (3)0.2461 (8)0.357 (2)0.030 (5)*
H5A0.851 (3)0.2073 (11)0.336 (3)0.053 (7)*
H5B0.954 (4)0.1781 (10)0.482 (3)0.055 (7)*
H5C0.860 (4)0.1394 (11)0.329 (3)0.064 (8)*
H6A0.215 (3)0.1286 (9)1.230 (3)0.048 (7)*
H6B0.075 (3)0.1342 (8)1.063 (3)0.037 (6)*
H6C0.204 (4)0.1835 (11)1.133 (3)0.054 (7)*
H80.491 (3)0.0799 (8)1.200 (2)0.034 (5)*
H10A0.757 (3)0.0269 (9)1.224 (3)0.046 (6)*
H10B0.782 (3)0.0005 (10)1.056 (3)0.045 (6)*
H10C0.888 (3)0.0486 (9)1.116 (3)0.042 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ga10.01474 (8)0.01490 (8)0.01408 (8)0.00243 (5)0.00237 (5)0.00118 (5)
Cl10.02214 (17)0.01832 (16)0.02242 (16)0.00162 (13)0.00158 (13)0.00144 (13)
O10.0231 (5)0.0175 (5)0.0226 (5)0.0047 (4)0.0057 (4)0.0048 (4)
O20.0273 (6)0.0289 (6)0.0161 (5)0.0105 (5)0.0069 (4)0.0044 (4)
N10.0191 (6)0.0235 (6)0.0297 (7)0.0033 (5)0.0093 (5)0.0033 (5)
N20.0222 (6)0.0201 (6)0.0206 (6)0.0068 (5)0.0003 (5)0.0000 (5)
C10.0397 (10)0.0211 (8)0.0289 (8)0.0059 (7)0.0005 (8)0.0076 (7)
C20.0285 (8)0.0162 (6)0.0170 (6)0.0013 (6)0.0018 (6)0.0004 (5)
C30.0312 (8)0.0255 (8)0.0203 (7)0.0048 (6)0.0044 (6)0.0065 (6)
C40.0191 (7)0.0292 (8)0.0201 (7)0.0064 (6)0.0036 (5)0.0000 (6)
C50.0264 (9)0.0566 (13)0.0457 (11)0.0035 (9)0.0150 (9)0.0169 (10)
C60.0335 (9)0.0399 (10)0.0222 (8)0.0052 (8)0.0119 (7)0.0051 (7)
C70.0244 (7)0.0224 (7)0.0177 (7)0.0035 (6)0.0053 (6)0.0008 (5)
C80.0263 (8)0.0272 (8)0.0175 (7)0.0020 (6)0.0026 (6)0.0082 (6)
C90.0212 (7)0.0155 (6)0.0220 (7)0.0018 (5)0.0034 (6)0.0029 (5)
C100.0307 (9)0.0297 (9)0.0296 (9)0.0063 (7)0.0052 (7)0.0087 (7)
C110.0189 (17)0.0374 (19)0.0250 (18)0.0087 (14)0.0043 (14)0.0039 (16)
C120.026 (3)0.028 (3)0.028 (2)0.011 (2)0.005 (2)0.002 (2)
C11B0.018 (2)0.023 (2)0.023 (3)0.0046 (18)0.006 (2)0.0000 (19)
C12B0.018 (4)0.024 (4)0.028 (3)0.006 (2)0.001 (3)0.002 (3)
Geometric parameters (Å, º) top
Ga1—O21.9078 (10)C1—H1A0.94 (2)
Ga1—O11.9168 (10)C1—H1B0.90 (3)
Ga1—N11.9897 (13)C1—H1C0.94 (3)
Ga1—N22.0039 (12)C3—H30.918 (19)
Ga1—Cl12.2237 (4)C5—H5A0.92 (3)
O1—C21.3016 (18)C5—H5B0.88 (3)
O2—C71.2998 (17)C5—H5C1.05 (3)
N1—C41.312 (2)C6—H6A0.92 (2)
N1—C11B1.483 (4)C6—H6B0.95 (2)
N1—C111.500 (3)C6—H6C0.95 (3)
N2—C91.3106 (19)C8—H80.903 (16)
N2—C121.439 (8)C10—H10A0.98 (2)
N2—C12B1.531 (11)C10—H10B0.91 (2)
C1—C21.504 (2)C10—H10C0.90 (2)
C2—C31.368 (2)C11—H11A0.9700
C3—C41.416 (2)C11—H11B0.9700
C4—C51.507 (2)C11B—H11D0.9700
C6—C71.503 (2)C11B—H11C0.9700
C7—C81.370 (2)C12—H12B0.9700
C8—C91.418 (2)C12—H12A0.9700
C9—C101.508 (2)C12B—H12C0.9700
C11—C121.520 (9)C12B—H12D0.9700
C11B—C12B1.529 (13)
O2—Ga1—O183.90 (4)C2—C1—H1A111.1 (15)
O2—Ga1—N1151.66 (6)C2—C1—H1B110.6 (17)
O1—Ga1—N190.88 (5)C2—C1—H1C113.9 (17)
O2—Ga1—N290.56 (5)H1A—C1—H1B106 (2)
O1—Ga1—N2153.22 (5)H1A—C1—H1C107 (2)
N1—Ga1—N281.65 (5)H1B—C1—H1C108 (2)
O2—Ga1—Cl1104.61 (4)C2—C3—H3116.6 (13)
O1—Ga1—Cl1103.76 (3)C4—C3—H3117.6 (13)
N1—Ga1—Cl1103.70 (4)C4—C5—H5A108.0 (14)
N2—Ga1—Cl1103.00 (4)C4—C5—H5B110.6 (17)
C2—O1—Ga1127.85 (10)C4—C5—H5C110.0 (16)
C7—O2—Ga1128.21 (10)H5A—C5—H5B106 (2)
C4—N1—C11B121.9 (2)H5A—C5—H5C112 (2)
C4—N1—C11118.06 (18)H5B—C5—H5C110 (2)
C4—N1—Ga1127.65 (11)C7—C6—H6A113.5 (14)
C11B—N1—Ga1108.72 (19)C7—C6—H6B106.3 (14)
C11—N1—Ga1112.76 (14)C7—C6—H6C109.0 (17)
C9—N2—C12122.0 (3)H6A—C6—H6B109 (2)
C9—N2—C12B120.5 (4)H6A—C6—H6C110 (2)
C9—N2—Ga1127.83 (11)H6B—C6—H6C109 (2)
C12—N2—Ga1109.5 (3)C7—C8—H8117.5 (14)
C12B—N2—Ga1111.0 (4)C9—C8—H8116.8 (14)
O1—C2—C3125.57 (14)C9—C10—H10A112.8 (13)
O1—C2—C1114.33 (14)C9—C10—H10B111.7 (15)
C3—C2—C1120.10 (14)C9—C10—H10C110.5 (14)
C2—C3—C4125.75 (14)H10A—C10—H10B110 (2)
N1—C4—C3122.07 (14)H10A—C10—H10C106 (2)
N1—C4—C5120.39 (15)H10B—C10—H10C105 (2)
C3—C4—C5117.54 (15)N1—C11—H11A109.82
O2—C7—C8125.85 (14)N1—C11—H11B109.82
O2—C7—C6113.50 (14)H11A—C11—H11B108.26
C8—C7—C6120.64 (14)N1—C11B—H11C111.08
C7—C8—C9125.65 (14)N1—C11B—H11D111.08
N2—C9—C8121.70 (13)H11C—C11B—H11D109.05
N2—C9—C10121.15 (15)N2—C12—H12A110.41
C8—C9—C10117.14 (14)N2—C12—H12B110.41
N1—C11—C12109.3 (4)H12A—C12—H12B108.62
N2—C12—C11106.6 (5)N2—C12B—H12C109.56
N1—C11B—C12B103.4 (6)N2—C12B—H12D109.56
C11B—C12B—N2110.5 (7)H12C—C12B—H12D108.11
O2—Ga1—O1—C2157.15 (12)C1—C2—C3—C4178.84 (15)
N1—Ga1—O1—C25.08 (12)C11B—N1—C4—C3161.9 (4)
N2—Ga1—O1—C278.11 (16)C11—N1—C4—C3166.1 (3)
Cl1—Ga1—O1—C299.26 (12)Ga1—N1—C4—C31.3 (2)
O1—Ga1—O2—C7158.61 (13)C11B—N1—C4—C518.8 (5)
N1—Ga1—O2—C778.14 (17)C11—N1—C4—C513.2 (4)
N2—Ga1—O2—C74.87 (13)Ga1—N1—C4—C5177.99 (14)
Cl1—Ga1—O2—C798.72 (13)C2—C3—C4—N12.2 (3)
O2—Ga1—N1—C480.41 (18)C2—C3—C4—C5177.04 (17)
O1—Ga1—N1—C41.67 (14)Ga1—O2—C7—C84.3 (2)
N2—Ga1—N1—C4155.85 (15)Ga1—O2—C7—C6176.30 (12)
Cl1—Ga1—N1—C4102.72 (13)O2—C7—C8—C90.2 (3)
O2—Ga1—N1—C11B114.6 (4)C6—C7—C8—C9179.58 (16)
O1—Ga1—N1—C11B166.7 (4)C12—N2—C9—C8170.7 (5)
N2—Ga1—N1—C11B39.2 (4)C12B—N2—C9—C8168.4 (5)
Cl1—Ga1—N1—C11B62.3 (4)Ga1—N2—C9—C81.1 (2)
O2—Ga1—N1—C1185.1 (3)C12—N2—C9—C109.4 (5)
O1—Ga1—N1—C11163.8 (3)C12B—N2—C9—C1011.5 (5)
N2—Ga1—N1—C119.6 (3)Ga1—N2—C9—C10178.95 (12)
Cl1—Ga1—N1—C1191.8 (3)C7—C8—C9—N21.4 (2)
O2—Ga1—N2—C93.36 (13)C7—C8—C9—C10178.58 (16)
O1—Ga1—N2—C980.85 (17)C4—N1—C11—C12178.8 (4)
N1—Ga1—N2—C9156.00 (14)C11B—N1—C11—C1273.0 (6)
Cl1—Ga1—N2—C9101.77 (13)Ga1—N1—C11—C1214.2 (6)
O2—Ga1—N2—C12174.0 (4)C9—N2—C12—C11139.9 (4)
O1—Ga1—N2—C12108.5 (4)C12B—N2—C12—C1149 (2)
N1—Ga1—N2—C1233.4 (4)Ga1—N2—C12—C1148.8 (6)
Cl1—Ga1—N2—C1268.9 (4)N1—C11—C12—N240.3 (7)
O2—Ga1—N2—C12B166.9 (5)C4—N1—C11B—C12B140.6 (5)
O1—Ga1—N2—C12B89.5 (5)C11—N1—C11B—C12B50.1 (7)
N1—Ga1—N2—C12B14.3 (5)Ga1—N1—C11B—C12B53.4 (6)
Cl1—Ga1—N2—C12B87.9 (5)N1—C11B—C12B—N241.1 (9)
Ga1—O1—C2—C35.8 (2)C9—N2—C12B—C11B176.9 (5)
Ga1—O1—C2—C1174.47 (11)C12—N2—C12B—C11B76 (2)
O1—C2—C3—C41.4 (3)Ga1—N2—C12B—C11B11.9 (9)

Experimental details

Crystal data
Chemical formula[Ga(C12H18N2O2)Cl]
Mr327.45
Crystal system, space groupMonoclinic, P21/n
Temperature (K)163
a, b, c (Å)7.2163 (6), 24.102 (2), 8.0669 (7)
β (°) 101.776 (1)
V3)1373.5 (2)
Z4
Radiation typeMo Kα
µ (mm1)2.19
Crystal size (mm)0.33 × 0.20 × 0.12
Data collection
DiffractometerBruker SMART CCD
diffractometer
Absorption correctionEmpirical (using intensity measurements)
(SADABS; Bruker, 1998)
Tmin, Tmax0.531, 0.779
No. of measured, independent and
observed [I > 2σ(I)] reflections
14190, 3298, 2992
Rint0.024
(sin θ/λ)max1)0.667
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.020, 0.051, 1.08
No. of reflections3298
No. of parameters239
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.32, 0.25

Computer programs: SMART (Bruker, 1998), SMART, SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL.

 

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