supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportcited insimilar papers buy article online

Acta Cryst. (2007). E63, m1438    [ doi:10.1107/S1600536807018144 ]

[13,27-Dimethyl-3,6,9,17,20,23-hexaazatricyclo[23.3.1.111,15]triaconta-1(29),2,9,11,13,15(30),16,23,25,27-decaene-29,30-diol-[kappa]5N3,N6,N9,O29,O30]bis(nitrato-[kappa]2O,O')gadolinium(III) nitrate monohydrate

X.-L. Hu, L. Qiu, J. Yuan and Z.-Q. Pan

Abstract top

The Gd atom in the title title complex, [Gd(NO3)2(C26H34N6O2)]NO3·H2O, exhibits a nine-coordinate distorted tricapped trigonal prismatic coordination geometry. The water molecule is disordered, with restrained occupancy factors of 0.4 and 0.6, with one component lying on a twofold rotation axis.

Comment top

Lanthanide macrocyclic complexes have been received extensive attention, owing to their many possible applications in biological systems, material science and chemical processes (Alexander, 1995;Hu et al., 2003; Hu et al., 2004). A series of lanthanide(III) complexes with macrocyclic Schiff bases have synthesized by one step template condensation of 2,6-diformyl- 4-chlorophenol with 1,5-diamino-3-azapentane in the presence of lanthanide ions (Alexander, 1995). Guerriero et al. (1987) and Bunzli et al. (1988) have reported the crystal structures of the Tb(III) and Eu(III) complexes in which the central ion is nine-coordinate, being bound to five donor atoms from the cyclic polydentate ligand and to four O atoms of two bidentae nitrates.

The title complex (I) (Fig. 1), which is synthesized by template reaction of 2,6-diformyl-4-methylphenol with 1,5-diamino-3-azapentane in the presence of gadolinium(III) nitrate, exhibits a similar coordinate geometry (Fig. 2). Gd1 is encaptured with in the macrocyclic ligand which provided five donor atoms (the two O atoms O1, O2 from the phenolates and the three N atoms N1, N2, N3 from one end of the macrocycle). The ninefold coordination is completed around Gd1 by two bidentate nitrates which locate on the opposite sides of the bisphenoidal positions. The third nitrate is ionic. At the free end of the macrocycle, a further five-membered imidazoling rings is formed by contraction, this makes the ligand more compact hence allowing a more appropriate spatial arrangement of the donor atoms of the macrocyclic ligand around the lanthanide ions. The coordination polyhedron can be described as a distorted tricapped trigonal prism in which N2, O4 and O7 are the caps, as show in Fig.2.

Related literature top

For related literature, see: Alexander (1995); Bunzli & Moret (1988); Guerriero et al. (1987); Hu et al. (2003, 2004).

Experimental top

To a methanolic solution (20 ml) of 2,6-diformyl-4-methylphenol(1 mmol) and Gd(NO3)3.6H2O (0.5 mmol), 1,5-diamino-3-azapentane (1 mmol) was added dropwise. After refluxing 3 h, the solvent was removed. Yellow solid was recrystallized in acetonitrile and then yellow block crystals suitable for X-ray analysis were obtained.

Refinement top

The carbon-bound H atoms were generated geometrically (C–H 0.93 to 0.97 Å) and were included in the refinement in the riding model approximation, with U(H) set to 1.2Ueq(C). The water H atom was located in a difference Fourier map, and was refined with an O–H distance restraint of 0.85±0.01 Å; its temperature factor was refined.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot of (I). Displacement ellipsoids are drawn at the 30% probability level.
[Figure 2] Fig. 2. Coordination polyhedron in (I).
(13,27-Dimethyl-3,6,9,17,20,23-hexaazatricyclo[23.3.1.111,15]triaconta- 1(29),2,9,11,13,15 (30),16,23,25,27-decaene-29,30-diol- N3,N6,N9,O29,O30)bis(nitrato-κ2O,O')gadolinium(III) nitrate hydrate top
Crystal data top
[Gd(NO3)2(C26H34N6O2)]NO3·H2OF(000) = 3320
Mr = 823.89Dx = 1.628 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 5110 reflections
a = 23.764 (3) Åθ = 2.6–25.0°
b = 14.298 (3) ŵ = 2.05 mm−1
c = 19.804 (2) ÅT = 291 K
β = 91.769 (2)°Block, yellow
V = 6724.5 (13) Å30.30 × 0.26 × 0.24 mm
Z = 8
Data collection top
Bruker SMART CCD area-detector
diffractometer		6596 independent reflections
Radiation source: sealed tube4171 reflections with I > 2σ(I)
graphiteRint = 0.046
φ and ω scansθmax = 26.0°, θmin = 2.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		h = −29→22
Tmin = 0.55, Tmax = 0.61k = −16→17
19136 measured reflectionsl = −23→24
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)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107H-atom parameters constrained
S = 0.98 w = 1/[σ2(Fo2) + (0.052P)2]
where P = (Fo2 + 2Fc2)/3
6596 reflections(Δ/σ)max < 0.001
440 parametersΔρmax = 0.41 e Å−3
0 restraintsΔρmin = −1.38 e Å−3
Crystal data top
[Gd(NO3)2(C26H34N6O2)]NO3·H2OV = 6724.5 (13) Å3
Mr = 823.89Z = 8
Monoclinic, C2/cMo Kα radiation
a = 23.764 (3) ŵ = 2.05 mm−1
b = 14.298 (3) ÅT = 291 K
c = 19.804 (2) Å0.30 × 0.26 × 0.24 mm
β = 91.769 (2)°
Data collection top
Bruker SMART CCD area-detector
diffractometer		6596 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		4171 reflections with I > 2σ(I)
Tmin = 0.55, Tmax = 0.61Rint = 0.046
19136 measured reflectionsθmax = 26.0°
Refinement top
R[F2 > 2σ(F2)] = 0.049H-atom parameters constrained
wR(F2) = 0.107Δρmax = 0.41 e Å−3
S = 0.98Δρmin = −1.38 e Å−3
6596 reflectionsAbsolute structure: ?
440 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
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*/UeqOcc. (<1)
C10.2695 (2)0.9536 (4)0.1213 (3)0.0501 (13)
C20.2875 (2)1.0154 (4)0.0702 (3)0.0563 (14)
C30.3425 (3)1.0095 (4)0.0459 (3)0.0585 (14)
H30.35431.05260.01420.070*
C40.3791 (3)0.9403 (4)0.0685 (3)0.0570 (14)
C50.3604 (3)0.8761 (4)0.1157 (3)0.0589 (15)
H50.38430.82790.12980.071*
C60.3075 (3)0.8820 (4)0.1422 (3)0.0563 (14)
C70.4394 (2)0.9327 (5)0.0409 (3)0.0607 (15)
H7A0.46590.96010.07270.091*
H7B0.44090.9652−0.00140.091*
H7C0.44870.86800.03440.091*
C80.2520 (3)1.0863 (4)0.0406 (3)0.0652 (16)
H80.26921.12610.01030.078*
C90.1757 (3)1.1865 (4)0.0145 (3)0.0593 (15)
H9A0.19141.1923−0.02990.071*
H9B0.18511.24260.04000.071*
C100.1122 (3)1.1764 (4)0.0078 (3)0.0611 (16)
H10A0.09581.2350−0.00760.073*
H10B0.10281.1286−0.02540.073*
C110.0258 (3)1.1483 (4)0.0724 (3)0.0575 (15)
H11A0.01101.21130.06860.069*
H11B0.01141.11240.03410.069*
C120.0074 (3)1.1057 (4)0.1351 (3)0.0569 (15)
H12A−0.03341.10620.13610.068*
H12B0.02201.14110.17350.068*
C13−0.0081 (2)0.9434 (4)0.1513 (3)0.0542 (14)
H13−0.04450.96260.16020.065*
C140.0023 (2)0.8441 (4)0.1526 (3)0.0537 (13)
C15−0.0424 (3)0.7853 (4)0.1679 (3)0.0626 (15)
H15−0.07630.81340.17860.075*
C16−0.0405 (2)0.6898 (4)0.1684 (3)0.0536 (13)
C170.0090 (3)0.6498 (4)0.1495 (3)0.0586 (15)
H170.01110.58490.14720.070*
C180.0560 (3)0.7014 (4)0.1337 (3)0.0570 (14)
C190.0547 (2)0.8007 (4)0.1346 (3)0.0504 (13)
C20−0.0906 (3)0.6320 (4)0.1876 (3)0.0613 (16)
H20A−0.11940.67240.20390.092*
H20B−0.07940.58850.22230.092*
H20C−0.10480.59840.14870.092*
C210.1067 (3)0.6533 (4)0.1148 (3)0.0512 (13)
H210.10630.58820.11610.061*
C220.2031 (2)0.6402 (4)0.0824 (3)0.0548 (14)
H22A0.20520.62900.03420.066*
H22B0.20230.58020.10520.066*
C230.2554 (2)0.6978 (4)0.1079 (3)0.0516 (13)
H23A0.28680.65560.11660.062*
H23B0.26610.74120.07300.062*
C240.2306 (3)0.6971 (4)0.2291 (3)0.0546 (14)
H24A0.25900.65060.24050.065*
H24B0.19420.66660.22410.065*
C250.2295 (3)0.7747 (4)0.2825 (3)0.0647 (16)
H25A0.19120.79390.29100.078*
H25B0.24760.75450.32460.078*
C260.2897 (2)0.8117 (4)0.1911 (3)0.0499 (13)
H260.32240.77480.20640.060*
Gd10.132602 (11)0.996866 (19)0.112967 (14)0.04773 (10)
N10.0281 (2)1.0091 (3)0.1389 (2)0.0551 (11)
N20.0895 (2)1.1511 (3)0.0718 (3)0.0590 (13)
H20.10091.19580.10200.071*
N30.2000 (2)1.1025 (3)0.0500 (2)0.0542 (12)
N40.2619 (2)0.8522 (3)0.2508 (2)0.0554 (11)
H4A0.23850.89890.23790.067*
H4B0.28780.87520.28050.067*
N50.2444 (2)0.7482 (4)0.1676 (3)0.0641 (13)
N60.1521 (2)0.6931 (3)0.0965 (2)0.0584 (12)
H6A0.15270.75300.09240.070*
N70.1260 (2)0.8939 (3)−0.0123 (2)0.0533 (11)
N80.1368 (2)1.0475 (4)0.2570 (3)0.0598 (12)
N90.1283 (2)0.3947 (4)0.1408 (3)0.0589 (13)
O10.22107 (16)0.9625 (3)0.15061 (18)0.0525 (9)
O20.09826 (15)0.8486 (2)0.12235 (18)0.0485 (8)
O30.09112 (17)0.9594 (3)−0.00056 (19)0.0583 (10)
O40.17109 (19)0.8926 (3)0.0223 (2)0.0637 (11)
O50.11340 (17)0.8315 (3)−0.0522 (2)0.0648 (11)
O60.13705 (18)1.1068 (3)0.2101 (2)0.0640 (11)
O70.13078 (17)0.9602 (3)0.2391 (2)0.0616 (10)
O80.1408 (2)1.0668 (3)0.3166 (3)0.0853 (14)
O90.14265 (19)0.3210 (3)0.1536 (2)0.0661 (12)
O100.15358 (18)0.4520 (3)0.1704 (2)0.0627 (11)
O110.0879 (2)0.4096 (3)0.1042 (2)0.0685 (12)
O1W0.00000.3603 (5)0.25000.069 (2)0.80
H1WA0.00810.30260.24740.083*0.40
H1WB0.01450.38960.21750.083*0.40
O2W0.8107 (3)0.9370 (5)0.1122 (3)0.0629 (17)0.60
H2WD0.84650.93830.11290.075*0.60
H2WB0.79810.99180.11890.075*0.60
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.048 (3)0.049 (3)0.053 (3)0.013 (2)−0.006 (2)0.011 (2)
C20.040 (3)0.055 (4)0.074 (4)0.009 (2)0.002 (3)0.003 (3)
C30.057 (3)0.052 (3)0.067 (3)0.007 (3)−0.001 (3)−0.003 (3)
C40.050 (3)0.062 (4)0.058 (3)0.010 (3)−0.004 (3)0.013 (3)
C50.054 (4)0.057 (3)0.065 (3)0.007 (3)−0.004 (3)0.010 (3)
C60.050 (3)0.057 (3)0.062 (3)0.007 (3)0.005 (3)−0.004 (3)
C70.035 (3)0.074 (4)0.073 (4)0.013 (3)0.007 (3)0.010 (3)
C80.072 (5)0.064 (4)0.059 (3)0.009 (3)−0.007 (3)−0.009 (3)
C90.059 (4)0.061 (4)0.056 (3)0.013 (3)−0.010 (3)−0.007 (3)
C100.066 (4)0.053 (3)0.063 (4)−0.004 (3)−0.016 (3)−0.014 (3)
C110.060 (4)0.052 (3)0.059 (3)−0.007 (3)−0.019 (3)0.000 (3)
C120.049 (3)0.054 (3)0.067 (4)−0.007 (3)−0.008 (3)0.024 (3)
C130.035 (3)0.060 (3)0.067 (3)−0.004 (3)0.001 (2)0.014 (3)
C140.037 (3)0.064 (4)0.061 (3)0.003 (3)0.005 (2)0.011 (3)
C150.054 (4)0.066 (4)0.068 (4)0.002 (3)0.008 (3)0.026 (3)
C160.046 (3)0.060 (3)0.055 (3)0.014 (3)0.010 (2)0.013 (3)
C170.055 (4)0.062 (4)0.059 (3)0.005 (3)0.005 (3)0.006 (3)
C180.063 (4)0.053 (3)0.055 (3)−0.002 (3)0.000 (3)0.006 (2)
C190.036 (3)0.046 (3)0.069 (3)−0.002 (2)0.003 (2)0.005 (2)
C200.061 (4)0.053 (3)0.071 (4)0.025 (3)0.027 (3)0.018 (3)
C210.061 (4)0.033 (3)0.059 (3)0.001 (2)−0.006 (3)0.008 (2)
C220.052 (4)0.057 (3)0.056 (3)−0.008 (3)0.017 (3)0.007 (3)
C230.039 (3)0.059 (3)0.057 (3)−0.009 (2)0.013 (2)0.003 (3)
C240.046 (3)0.063 (4)0.056 (3)0.001 (3)0.004 (3)−0.018 (3)
C250.056 (4)0.069 (4)0.069 (4)0.020 (3)0.009 (3)−0.005 (3)
C260.030 (3)0.064 (3)0.055 (3)−0.003 (2)−0.003 (2)−0.006 (2)
Gd10.03673 (14)0.04502 (15)0.06105 (16)0.00045 (12)−0.00490 (10)0.00840 (13)
N10.048 (3)0.050 (3)0.067 (3)−0.009 (2)−0.005 (2)0.020 (2)
N20.057 (3)0.047 (3)0.071 (3)−0.004 (2)−0.028 (2)0.007 (2)
N30.043 (3)0.060 (3)0.059 (3)0.007 (2)−0.007 (2)−0.014 (2)
N40.046 (3)0.060 (3)0.060 (3)−0.001 (2)−0.006 (2)0.009 (2)
N50.061 (3)0.065 (3)0.066 (3)0.000 (3)0.000 (3)0.001 (2)
N60.066 (3)0.046 (3)0.063 (3)−0.002 (2)0.004 (3)0.004 (2)
N70.048 (3)0.050 (3)0.063 (3)0.002 (2)0.011 (2)0.002 (2)
N80.049 (3)0.067 (3)0.064 (3)0.009 (3)0.012 (2)0.008 (3)
N90.054 (3)0.057 (3)0.065 (3)−0.001 (2)−0.022 (2)0.026 (2)
O10.048 (2)0.053 (2)0.057 (2)0.0023 (17)0.0058 (18)0.0030 (17)
O20.047 (2)0.0388 (18)0.061 (2)0.0012 (16)0.0111 (17)0.0042 (15)
O30.055 (2)0.062 (2)0.057 (2)−0.008 (2)−0.0115 (18)0.0004 (18)
O40.062 (3)0.064 (3)0.065 (2)0.006 (2)0.004 (2)0.0013 (19)
O50.061 (3)0.067 (3)0.066 (3)−0.004 (2)0.003 (2)0.036 (2)
O60.063 (3)0.065 (3)0.064 (2)0.008 (2)−0.005 (2)0.014 (2)
O70.054 (3)0.067 (3)0.065 (2)0.010 (2)0.0086 (19)0.026 (2)
O80.064 (3)0.075 (3)0.118 (4)0.006 (2)0.019 (3)0.005 (3)
O90.066 (3)0.069 (3)0.062 (2)0.021 (2)−0.018 (2)−0.014 (2)
O100.062 (3)0.058 (2)0.066 (2)−0.015 (2)−0.022 (2)0.021 (2)
O110.067 (3)0.070 (3)0.067 (3)−0.011 (2)−0.017 (2)0.017 (2)
O1W0.067 (5)0.072 (5)0.071 (5)0.0000.016 (4)0.000
O2W0.047 (4)0.067 (4)0.074 (4)0.005 (3)0.002 (3)0.005 (3)
Geometric parameters (Å, °) top
C1—O11.311 (6)C21—N61.284 (8)
C1—C61.417 (7)C21—H210.9300
C1—C21.421 (8)C22—N61.462 (8)
C2—C31.408 (8)C22—C231.563 (8)
C2—C81.433 (8)C22—H22A0.9700
C3—C41.383 (8)C22—H22B0.9700
C3—H30.9300C23—N51.415 (7)
C4—C51.392 (8)C23—H23A0.9700
C4—C71.552 (8)C23—H23B0.9700
C5—C61.380 (8)C24—N51.465 (8)
C5—H50.9300C24—C251.533 (8)
C6—C261.467 (8)C24—H24A0.9700
C7—H7A0.9600C24—H24B0.9700
C7—H7B0.9600C25—N41.497 (8)
C7—H7C0.9600C25—H25A0.9700
C8—N31.275 (8)C25—H25B0.9700
C8—H80.9300C26—N51.473 (7)
C9—N31.499 (7)C26—N41.490 (7)
C9—C101.516 (8)C26—H260.9800
C9—H9A0.9700Gd1—O12.263 (4)
C9—H9B0.9700Gd1—O22.281 (3)
C10—N21.439 (8)Gd1—O62.483 (4)
C10—H10A0.9700Gd1—O32.485 (4)
C10—H10B0.9700Gd1—O42.527 (4)
C11—C121.462 (8)Gd1—O72.553 (4)
C11—N21.515 (8)Gd1—N22.554 (4)
C11—H11A0.9700Gd1—N32.555 (5)
C11—H11B0.9700Gd1—N12.558 (5)
C12—N11.467 (7)Gd1—N72.884 (5)
C12—H12A0.9700Gd1—N82.941 (6)
C12—H12B0.9700N2—H20.9100
C13—N11.302 (7)N4—H4A0.9000
C13—C141.442 (8)N4—H4B0.9000
C13—H130.9300N6—H6A0.8600
C14—C151.394 (8)N7—O51.223 (6)
C14—C191.446 (8)N7—O41.254 (6)
C15—C161.365 (8)N7—O31.277 (6)
C15—H150.9300N8—O81.213 (7)
C16—C171.371 (8)N8—O61.258 (6)
C16—C201.507 (8)N8—O71.304 (7)
C17—C181.383 (9)N9—O91.133 (6)
C17—H170.9300N9—O101.164 (6)
C18—C191.420 (8)N9—O111.204 (6)
C18—C211.445 (9)N9—O1W3.824 (6)
C19—O21.271 (6)O1W—H1WA0.8499
C20—H20A0.9600O1W—H1WB0.8501
C20—H20B0.9600O2W—H2WD0.8499
C20—H20C0.9600O2W—H2WB0.8500
O1—C1—C6120.1 (5)N5—C26—H26109.3
O1—C1—C2122.9 (5)N4—C26—H26109.3
C6—C1—C2117.0 (5)O1—Gd1—O295.90 (13)
C3—C2—C1120.6 (5)O1—Gd1—O682.25 (13)
C3—C2—C8116.4 (6)O2—Gd1—O6122.13 (13)
C1—C2—C8123.0 (6)O1—Gd1—O3126.15 (14)
C4—C3—C2120.9 (6)O2—Gd1—O374.96 (13)
C4—C3—H3119.5O6—Gd1—O3147.48 (13)
C2—C3—H3119.5O1—Gd1—O475.71 (14)
C3—C4—C5118.5 (6)O2—Gd1—O469.41 (13)
C3—C4—C7120.9 (5)O6—Gd1—O4156.35 (14)
C5—C4—C7120.5 (5)O3—Gd1—O451.10 (14)
C6—C5—C4121.9 (5)O1—Gd1—O771.15 (13)
C6—C5—H5119.0O2—Gd1—O773.31 (14)
C4—C5—H5119.0O6—Gd1—O751.25 (14)
C5—C6—C1120.9 (5)O3—Gd1—O7145.32 (14)
C5—C6—C26119.6 (5)O4—Gd1—O7126.28 (14)
C1—C6—C26119.5 (5)O1—Gd1—N2130.66 (15)
C4—C7—H7A109.5O2—Gd1—N2133.42 (14)
C4—C7—H7B109.5O6—Gd1—N273.01 (14)
H7A—C7—H7B109.5O3—Gd1—N275.73 (15)
C4—C7—H7C109.5O4—Gd1—N2115.63 (16)
H7A—C7—H7C109.5O7—Gd1—N2118.06 (16)
H7B—C7—H7C109.5O1—Gd1—N372.45 (14)
N3—C8—C2129.1 (7)O2—Gd1—N3145.13 (14)
N3—C8—H8115.5O6—Gd1—N389.51 (14)
C2—C8—H8115.5O3—Gd1—N385.59 (14)
N3—C9—C10109.5 (5)O4—Gd1—N375.83 (14)
N3—C9—H9A109.8O7—Gd1—N3128.93 (14)
C10—C9—H9A109.8N2—Gd1—N365.50 (16)
N3—C9—H9B109.8O1—Gd1—N1147.86 (14)
C10—C9—H9B109.8O2—Gd1—N172.23 (13)
H9A—C9—H9B108.2O6—Gd1—N179.62 (15)
N2—C10—C9110.2 (5)O3—Gd1—N180.55 (15)
N2—C10—H10A109.6O4—Gd1—N1123.92 (15)
C9—C10—H10A109.6O7—Gd1—N176.80 (14)
N2—C10—H10B109.6N2—Gd1—N167.85 (15)
C9—C10—H10B109.6N3—Gd1—N1133.27 (14)
H10A—C10—H10B108.1O1—Gd1—N7101.41 (14)
C12—C11—N2110.1 (5)O2—Gd1—N765.53 (13)
C12—C11—H11A109.6O6—Gd1—N7171.41 (12)
N2—C11—H11A109.6O3—Gd1—N726.18 (13)
C12—C11—H11B109.6O4—Gd1—N725.71 (13)
N2—C11—H11B109.6O7—Gd1—N7137.25 (14)
H11A—C11—H11B108.2N2—Gd1—N798.95 (15)
C11—C12—N1109.1 (5)N3—Gd1—N784.27 (14)
C11—C12—H12A109.9N1—Gd1—N7100.38 (15)
N1—C12—H12A109.9O1—Gd1—N874.39 (14)
C11—C12—H12B109.9O2—Gd1—N898.69 (14)
N1—C12—H12B109.9O6—Gd1—N825.03 (13)
H12A—C12—H12B108.3O3—Gd1—N8158.56 (14)
N1—C13—C14126.9 (6)O4—Gd1—N8146.35 (14)
N1—C13—H13116.6O7—Gd1—N826.26 (14)
C14—C13—H13116.6N2—Gd1—N895.62 (16)
C15—C14—C13117.8 (5)N3—Gd1—N8108.96 (14)
C15—C14—C19117.5 (6)N1—Gd1—N878.01 (15)
C13—C14—C19124.5 (5)N7—Gd1—N8163.50 (15)
C16—C15—C14125.4 (6)C13—N1—C12117.8 (5)
C16—C15—H15117.3C13—N1—Gd1129.8 (4)
C14—C15—H15117.3C12—N1—Gd1112.3 (3)
C15—C16—C17116.3 (6)C10—N2—C11114.6 (4)
C15—C16—C20121.6 (5)C10—N2—Gd1109.9 (4)
C17—C16—C20122.1 (5)C11—N2—Gd1111.4 (3)
C16—C17—C18123.0 (6)C10—N2—H2106.8
C16—C17—H17118.5C11—N2—H2106.8
C18—C17—H17118.5Gd1—N2—H2106.8
C17—C18—C19120.8 (6)C8—N3—C9116.0 (6)
C17—C18—C21119.3 (5)C8—N3—Gd1126.1 (4)
C19—C18—C21119.9 (5)C9—N3—Gd1117.6 (4)
O2—C19—C18121.2 (5)C26—N4—C25107.0 (4)
O2—C19—C14122.0 (5)C26—N4—H4A110.3
C18—C19—C14116.8 (5)C25—N4—H4A110.3
C16—C20—H20A109.5C26—N4—H4B110.3
C16—C20—H20B109.5C25—N4—H4B110.3
H20A—C20—H20B109.5H4A—N4—H4B108.6
C16—C20—H20C109.5C23—N5—C24119.5 (5)
H20A—C20—H20C109.5C23—N5—C26115.2 (5)
H20B—C20—H20C109.5C24—N5—C26103.0 (4)
N6—C21—C18125.2 (5)C21—N6—C22122.3 (5)
N6—C21—H21117.4C21—N6—H6A118.9
C18—C21—H21117.4C22—N6—H6A118.9
N6—C22—C23108.7 (5)O5—N7—O4122.1 (5)
N6—C22—H22A110.0O5—N7—O3120.3 (5)
C23—C22—H22A110.0O4—N7—O3117.4 (5)
N6—C22—H22B110.0O5—N7—Gd1159.1 (4)
C23—C22—H22B110.0O4—N7—Gd161.0 (3)
H22A—C22—H22B108.3O3—N7—Gd159.2 (3)
N5—C23—C22111.9 (5)O8—N8—O6124.3 (6)
N5—C23—H23A109.2O8—N8—O7119.2 (5)
C22—C23—H23A109.2O6—N8—O7116.5 (5)
N5—C23—H23B109.2O8—N8—Gd1177.1 (4)
C22—C23—H23B109.2O6—N8—Gd156.7 (3)
H23A—C23—H23B107.9O7—N8—Gd160.0 (3)
N5—C24—C25102.8 (5)O9—N9—O10113.2 (5)
N5—C24—H24A111.2O9—N9—O11121.9 (6)
C25—C24—H24A111.2O10—N9—O11124.6 (5)
N5—C24—H24B111.2O9—N9—O1W89.7 (4)
C25—C24—H24B111.2O10—N9—O1W102.3 (4)
H24A—C24—H24B109.1O11—N9—O1W74.2 (3)
N4—C25—C24103.1 (5)C1—O1—Gd1134.0 (3)
N4—C25—H25A111.1C19—O2—Gd1144.3 (3)
C24—C25—H25A111.1N7—O3—Gd194.6 (3)
N4—C25—H25B111.1N7—O4—Gd193.3 (3)
C24—C25—H25B111.1N8—O6—Gd198.3 (4)
H25A—C25—H25B109.1N8—O7—Gd193.7 (3)
C6—C26—N5115.8 (5)N9—O1W—H1WA84.5
C6—C26—N4113.7 (5)H1WA—O1W—H1WB109.5
N5—C26—N498.7 (4)H2WD—O2W—H2WB109.5
C6—C26—H26109.3
Table 1
Selected geometric parameters (Å) top
Gd1—O12.263 (4)Gd1—O72.553 (4)
Gd1—O22.281 (3)Gd1—N22.554 (4)
Gd1—O62.483 (4)Gd1—N32.555 (5)
Gd1—O32.485 (4)Gd1—N12.558 (5)
Gd1—O42.527 (4)
Acknowledgements top

The work was supported by the Education Office of Hubei Province, People's Republic of China (No. D200515004) and the Natural Science Foundation of Hubei Province, People's Republic of China(No.2005ABA021)

references
References top

Alexander, V. (1995). Chem. Rev. 95, 273–342.

Bruker (2000). SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.

Bunzli, J.-C. G. & Moret, E. (1988). Inorg. Chim. Acta, 150, 133–139.

Guerriero, P., Casellato, U., Tamburini, S. & Vigato, P. A. (1987). Inorg. Chim. Acta, 129, 127–138.

Hu, X.-L., Li, Y.-Z. & Luo, Q.-H. (2003). J. Coord. Chem. 56, 1277–1283.

Hu, X.-L., Li, Y.-Z. & Luo, Q.-H. (2004). Polyhedron, 23, 49–53.