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Acta Crystallogr Sect E Struct Rep Online. 2008 June 1; 64(Pt 6): m789.
Published online 2008 May 10. doi:  10.1107/S1600536808012981
PMCID: PMC2961579

catena-Poly[[aqua­[3-(3-pyrid­yl)acrylato]gadolinium(III)]-bis­[μ-3-(3-pyrid­yl)acrylato]]

Abstract

In the title compound, [Gd(C8H6NO2)3(H2O)]n, the gadolinium(III) ion is coordinated by eight carboxyl­ate O atoms and one water mol­ecule. The carboxyl­ate ligands bridge pairs of gadolinium(III) ions, forming a zigzag chain along [100]. Hydrogen bonds link the chains into sheets parallel to (001).

Related literature

For related literature, see: Ayyappan et al. (2001 [triangle]); Gunning & Cahill (2005 [triangle]); Zhang et al. (2000 [triangle]). For related structures, see: Liu et al. (2004 [triangle], 2006 [triangle]); Zhou et al. (2004 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-0m789-scheme1.jpg

Experimental

Crystal data

  • [Gd(C8H6NO2)3(H2O)]
  • M r = 619.68
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m789-efi1.jpg
  • a = 6.2118 (7) Å
  • b = 12.7222 (14) Å
  • c = 15.6601 (18) Å
  • α = 111.741 (2)°
  • β = 90.309 (2)°
  • γ = 95.260 (2)°
  • V = 1143.7 (2) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 2.95 mm−1
  • T = 294 (2) K
  • 0.24 × 0.16 × 0.10 mm

Data collection

  • Bruker SMART 1000 diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2007 [triangle]) T min = 0.538, T max = 0.757
  • 5840 measured reflections
  • 3998 independent reflections
  • 3745 reflections with I > 2σ(I)
  • R int = 0.024

Refinement

  • R[F 2 > 2σ(F 2)] = 0.027
  • wR(F 2) = 0.070
  • S = 1.04
  • 3998 reflections
  • 324 parameters
  • 3 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 1.46 e Å−3
  • Δρmin = −2.22 e Å−3

Data collection: SMART (Bruker, 2007 [triangle]); cell refinement: SAINT (Bruker, 2007 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Bruker, 2007 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808012981/om2225sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808012981/om2225Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work was supported by the Natural Science Foundation of Guangxi (GKJ0639031), People’s Republic of China.

supplementary crystallographic information

Comment

The bifunctional ligand 3-pyridylacrylic acid (HTPA) is a potential multidentate ligand,and several types of complexes of HTPA have been studied (Ayyappan et al. ,2001; Gunning & Cahill, 2005; Zhang et al., 2000). Until now, however, only a few crystallographic studies of 4f-block metal complexes of HTPA have been reported (Liu et al., 2006; Liu et al., 2004; Zhou et al., 2004).

Here, we reported the synthesis and structure of the title complex, [Gd(TPA)3(H2O)]n (Fig.1), whose structure consists of a repeating unit of formula [Gd(TPA)3(H2O)]. Each GdIII centre is coordinated by eight carboxylate O atoms and one water molecule. The gadolinium(III) ions are joined into a coordination polymer chain along [100] (Fig.2), reinforced by O—H···O hydrogen bonds. Adjacent [100] chains are linked by O—H···N hydrogen bonds, forming sheets parallel to (001) (Fig.3).

Experimental

A mixture of Gd(NO3)3.6H2O (0.25 mmol, 0.110 g), 3-pyridylacrylic acid (1.25 mmol,0.186 g), H2O (14 ml) was sealed in a 25 ml Teflon-lined stainless reactor and heated at 438 K for four days under autogenous pressure, then followed by slow cooling to room temperature, when a few colourless crystals were obtained. Analysis:found C 46.55, H 3.28, N 6.85%; C24H20GdN3O7 requires C 46.48, H 3.23, N 6.78%.

Refinement

H atoms of the water molecules were located in a difference map and freely refined. H atoms bonded to C atoms were placed at calculated positions and treated using a riding-model approximation [C—H = 0.93Å and Uiso(H)= 1.2Ueq(C)].

Figures

Fig. 1.
A portion of the structure showing the coordination environment of the GdIII ion, with displacement ellipsoids at the 50% probability level. H atoms are shown as small spheres of arbitrary radii. [Symmetry codes: (a) -x,1-y,-z; (b)1-x,1-y,-z.]
Fig. 2.
Part of a chain structure along the a axis. All H atoms are omitted.
Fig. 3.
A packing diagram viewed along the a axis.

Crystal data

[Gd(C8H6NO2)3(H2O)]Z = 2
Mr = 619.68F000 = 610
Triclinic, P1Dx = 1.799 Mg m3
Hall symbol: -P 1Mo Kα radiation λ = 0.71073 Å
a = 6.2118 (7) ÅCell parameters from 5157 reflections
b = 12.7222 (14) Åθ = 2.7–25.9º
c = 15.6601 (18) ŵ = 2.95 mm1
α = 111.741 (2)ºT = 294 (2) K
β = 90.309 (2)ºBlock, colourless
γ = 95.260 (2)º0.24 × 0.16 × 0.10 mm
V = 1143.7 (2) Å3

Data collection

Bruker SMART 1000 diffractometer3998 independent reflections
Radiation source: fine-focus sealed tube3745 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.024
T = 294(2) Kθmax = 25.0º
[var phi] and ω scansθmin = 1.7º
Absorption correction: multi-scan(SADABS; Bruker, 2007)h = −3→7
Tmin = 0.538, Tmax = 0.757k = −15→14
5840 measured reflectionsl = −18→18

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.070  w = 1/[σ2(Fo2) + (0.0466P)2] where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
3998 reflectionsΔρmax = 1.46 e Å3
324 parametersΔρmin = −2.22 e Å3
3 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods

Special details

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)

xyzUiso*/Ueq
Gd10.24371 (2)0.472144 (12)0.075317 (10)0.01434 (8)
O10.0775 (4)0.2748 (2)0.01956 (19)0.0278 (6)
O2−0.0886 (4)0.38753 (19)−0.03041 (16)0.0186 (5)
O3−0.0667 (4)0.5066 (2)0.17142 (16)0.0234 (5)
O40.1965 (4)0.4402 (2)0.22361 (19)0.0347 (7)
O50.4079 (4)0.6447 (2)0.19685 (17)0.0253 (6)
O60.5959 (4)0.59101 (19)0.07279 (15)0.0192 (5)
O70.5409 (4)0.3842 (2)0.10173 (19)0.0235 (5)
H7A0.534 (8)0.319 (2)0.106 (4)0.09 (2)*
H7B0.657 (4)0.428 (3)0.122 (3)0.060 (17)*
N1−0.5448 (6)−0.1952 (3)−0.1445 (3)0.0363 (9)
N2−0.6805 (6)0.6840 (3)0.5098 (3)0.0473 (10)
N31.2920 (6)0.9676 (4)0.3726 (3)0.0581 (13)
C1−0.0758 (6)0.2899 (3)−0.0247 (2)0.0202 (7)
C2−0.2482 (6)0.1977 (3)−0.0705 (3)0.0270 (8)
H2−0.36450.2140−0.09950.032*
C3−0.2458 (6)0.0938 (3)−0.0724 (3)0.0281 (8)
H3−0.12400.0777−0.04660.034*
C4−0.4190 (6)0.0005 (3)−0.1120 (3)0.0263 (8)
C5−0.6180 (8)0.0145 (4)−0.1449 (4)0.0452 (12)
H5−0.64480.0852−0.14500.054*
C6−0.7752 (7)−0.0755 (4)−0.1773 (3)0.0431 (11)
H6−0.9080−0.0669−0.20030.052*
C7−0.7328 (7)−0.1786 (3)−0.1750 (3)0.0374 (10)
H7−0.8405−0.2391−0.19590.045*
C8−0.3917 (7)−0.1075 (3)−0.1140 (3)0.0321 (9)
H8−0.2593−0.1194−0.09300.039*
C90.0238 (6)0.4859 (3)0.2362 (3)0.0224 (8)
C10−0.0715 (6)0.5192 (3)0.3273 (3)0.0279 (8)
H10−0.00130.50530.37410.033*
C11−0.2553 (6)0.5686 (3)0.3448 (3)0.0274 (8)
H11−0.32500.57760.29560.033*
C12−0.3588 (6)0.6102 (3)0.4332 (3)0.0273 (8)
C13−0.2705 (7)0.6138 (4)0.5164 (3)0.0357 (9)
H13−0.13300.59150.51930.043*
C14−0.3881 (8)0.6504 (4)0.5937 (3)0.0455 (11)
H14−0.33190.65340.64980.055*
C15−0.5910 (8)0.6829 (4)0.5871 (3)0.0507 (13)
H15−0.67070.70560.63990.061*
C16−0.5622 (7)0.6482 (3)0.4349 (3)0.0351 (9)
H16−0.62030.64880.38020.042*
C170.5793 (6)0.6546 (3)0.1569 (2)0.0180 (7)
C180.7606 (6)0.7385 (3)0.2060 (3)0.0228 (8)
H180.89650.73080.18110.027*
C190.7388 (6)0.8243 (3)0.2838 (3)0.0257 (8)
H190.60230.82980.30830.031*
C200.9125 (6)0.9118 (3)0.3352 (3)0.0283 (8)
C210.8659 (7)1.0191 (3)0.3920 (3)0.0363 (10)
H210.72331.03660.39890.044*
C221.0313 (7)1.0991 (4)0.4378 (3)0.0458 (12)
H221.00291.17180.47600.055*
C231.2396 (8)1.0707 (5)0.4266 (4)0.0546 (14)
H231.35081.12590.45810.066*
C241.1281 (7)0.8911 (4)0.3285 (3)0.0426 (11)
H241.16050.81890.29080.051*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Gd10.01095 (11)0.01488 (11)0.01579 (12)0.00058 (7)0.00181 (7)0.00424 (8)
O10.0259 (14)0.0208 (14)0.0372 (16)−0.0015 (11)−0.0083 (12)0.0124 (12)
O20.0159 (12)0.0158 (12)0.0231 (13)−0.0012 (9)0.0005 (10)0.0065 (10)
O30.0171 (12)0.0325 (14)0.0211 (13)0.0011 (10)0.0028 (10)0.0109 (11)
O40.0255 (14)0.0538 (19)0.0321 (15)0.0163 (13)0.0089 (12)0.0217 (14)
O50.0185 (13)0.0281 (14)0.0229 (13)−0.0029 (11)0.0045 (10)0.0031 (11)
O60.0182 (12)0.0216 (13)0.0139 (12)0.0015 (10)0.0024 (9)0.0023 (10)
O70.0142 (12)0.0223 (14)0.0372 (15)0.0032 (10)0.0010 (11)0.0146 (12)
N10.043 (2)0.0181 (17)0.047 (2)−0.0042 (15)0.0030 (18)0.0124 (16)
N20.035 (2)0.049 (2)0.045 (2)0.0078 (18)0.0182 (18)0.0026 (19)
N30.0234 (19)0.050 (3)0.067 (3)−0.0048 (18)−0.0035 (19)−0.015 (2)
C10.0186 (18)0.0181 (18)0.0231 (19)0.0018 (14)0.0052 (15)0.0069 (15)
C20.0251 (19)0.021 (2)0.034 (2)−0.0027 (15)−0.0062 (17)0.0105 (17)
C30.0260 (19)0.022 (2)0.033 (2)0.0007 (15)−0.0018 (16)0.0066 (16)
C40.031 (2)0.0178 (18)0.028 (2)−0.0019 (15)−0.0004 (16)0.0072 (15)
C50.045 (3)0.027 (2)0.069 (3)−0.0043 (19)−0.016 (2)0.026 (2)
C60.037 (2)0.035 (2)0.058 (3)−0.0075 (19)−0.016 (2)0.021 (2)
C70.040 (2)0.030 (2)0.035 (2)−0.0119 (18)0.0007 (19)0.0070 (18)
C80.031 (2)0.024 (2)0.042 (2)0.0014 (17)−0.0012 (18)0.0132 (18)
C90.0168 (17)0.0264 (19)0.0230 (19)−0.0014 (15)0.0026 (14)0.0088 (16)
C100.027 (2)0.038 (2)0.0214 (19)0.0061 (17)0.0027 (15)0.0128 (17)
C110.0258 (19)0.032 (2)0.024 (2)0.0024 (16)0.0057 (16)0.0098 (17)
C120.028 (2)0.027 (2)0.024 (2)0.0011 (16)0.0069 (16)0.0054 (16)
C130.037 (2)0.039 (2)0.031 (2)0.0079 (18)0.0056 (18)0.0119 (19)
C140.061 (3)0.051 (3)0.022 (2)0.002 (2)0.007 (2)0.011 (2)
C150.054 (3)0.047 (3)0.036 (3)−0.001 (2)0.024 (2)0.000 (2)
C160.028 (2)0.040 (2)0.032 (2)0.0078 (18)0.0064 (17)0.0066 (19)
C170.0181 (17)0.0150 (17)0.0187 (18)0.0030 (13)−0.0004 (14)0.0034 (14)
C180.0191 (18)0.0217 (19)0.025 (2)0.0000 (14)0.0040 (15)0.0059 (16)
C190.0176 (17)0.027 (2)0.027 (2)0.0020 (15)0.0016 (15)0.0039 (16)
C200.0223 (19)0.024 (2)0.029 (2)−0.0014 (15)0.0008 (16)−0.0001 (16)
C210.028 (2)0.027 (2)0.039 (2)0.0052 (17)0.0007 (18)−0.0059 (18)
C220.042 (3)0.024 (2)0.051 (3)−0.0021 (19)0.000 (2)−0.008 (2)
C230.034 (3)0.039 (3)0.062 (4)−0.012 (2)−0.001 (2)−0.011 (2)
C240.026 (2)0.033 (2)0.047 (3)0.0035 (18)−0.0005 (19)−0.011 (2)

Geometric parameters (Å, °)

Gd1—O72.354 (2)C5—C61.371 (6)
Gd1—O6i2.410 (2)C5—H50.9300
Gd1—O2ii2.418 (2)C6—C71.373 (6)
Gd1—O32.424 (2)C6—H60.9300
Gd1—O52.440 (2)C7—H70.9300
Gd1—O12.454 (2)C8—H80.9300
Gd1—O42.515 (3)C9—C101.474 (5)
Gd1—O22.529 (2)C10—C111.335 (5)
Gd1—O62.552 (2)C10—H100.9300
O1—C11.245 (5)C11—C121.462 (5)
O2—C11.287 (4)C11—H110.9300
O2—Gd1ii2.418 (2)C12—C161.390 (6)
O3—C91.278 (4)C12—C131.394 (6)
O4—C91.249 (4)C13—C141.367 (6)
O5—C171.258 (4)C13—H130.9300
O6—C171.276 (4)C14—C151.377 (7)
O6—Gd1i2.410 (2)C14—H140.9300
O7—H7A0.853 (10)C15—H150.9300
O7—H7B0.850 (10)C16—H160.9300
N1—C71.323 (6)C17—C181.470 (5)
N1—C81.336 (5)C18—C191.319 (5)
N2—C151.334 (7)C18—H180.9300
N2—C161.341 (5)C19—C201.469 (5)
N3—C241.331 (6)C19—H190.9300
N3—C231.342 (7)C20—C211.384 (5)
C1—C21.475 (5)C20—C241.385 (6)
C2—C31.313 (5)C21—C221.366 (6)
C2—H20.9300C21—H210.9300
C3—C41.471 (5)C22—C231.370 (7)
C3—H30.9300C22—H220.9300
C4—C81.388 (5)C23—H230.9300
C4—C51.388 (6)C24—H240.9300
O7—Gd1—O6i77.79 (9)O2—C1—C2118.4 (3)
O7—Gd1—O2ii151.90 (8)O1—C1—Gd158.48 (19)
O6i—Gd1—O2ii86.86 (8)O2—C1—Gd162.02 (18)
O7—Gd1—O3123.56 (9)C2—C1—Gd1176.2 (3)
O6i—Gd1—O3151.93 (8)C3—C2—C1123.3 (4)
O2ii—Gd1—O379.63 (8)C3—C2—H2118.3
O7—Gd1—O586.21 (9)C1—C2—H2118.3
O6i—Gd1—O5118.78 (8)C2—C3—C4125.7 (4)
O2ii—Gd1—O580.71 (8)C2—C3—H3117.2
O3—Gd1—O583.35 (8)C4—C3—H3117.2
O7—Gd1—O181.11 (9)C8—C4—C5116.4 (4)
O6i—Gd1—O182.79 (9)C8—C4—C3120.0 (4)
O2ii—Gd1—O1120.49 (8)C5—C4—C3123.5 (3)
O3—Gd1—O183.09 (9)C6—C5—C4120.2 (4)
O5—Gd1—O1152.02 (9)C6—C5—H5119.9
O7—Gd1—O471.15 (9)C4—C5—H5119.9
O6i—Gd1—O4145.74 (8)C5—C6—C7118.8 (4)
O2ii—Gd1—O4127.39 (8)C5—C6—H6120.6
O3—Gd1—O452.65 (8)C7—C6—H6120.6
O5—Gd1—O473.78 (9)N1—C7—C6122.7 (4)
O1—Gd1—O478.53 (10)N1—C7—H7118.7
O7—Gd1—O2129.92 (8)C6—C7—H7118.7
O6i—Gd1—O279.03 (8)N1—C8—C4123.7 (4)
O2ii—Gd1—O268.19 (8)N1—C8—H8118.2
O3—Gd1—O273.13 (8)C4—C8—H8118.2
O5—Gd1—O2143.61 (8)O4—C9—O3120.4 (3)
O1—Gd1—O252.30 (8)O4—C9—C10119.5 (3)
O4—Gd1—O2110.31 (8)O3—C9—C10120.1 (3)
O7—Gd1—O670.08 (8)O4—C9—Gd162.80 (19)
O6i—Gd1—O667.09 (9)O3—C9—Gd158.70 (17)
O2ii—Gd1—O682.33 (8)C10—C9—Gd1167.6 (3)
O3—Gd1—O6133.93 (8)C11—C10—C9122.2 (4)
O5—Gd1—O651.95 (8)C11—C10—H10118.9
O1—Gd1—O6141.65 (8)C9—C10—H10118.9
O4—Gd1—O6113.50 (8)C10—C11—C12126.9 (4)
O2—Gd1—O6136.03 (7)C10—C11—H11116.5
O7—Gd1—C997.34 (10)C12—C11—H11116.5
O6i—Gd1—C9165.27 (10)C16—C12—C13117.0 (4)
O2ii—Gd1—C9102.81 (9)C16—C12—C11117.9 (4)
O3—Gd1—C926.77 (9)C13—C12—C11125.1 (4)
O5—Gd1—C974.26 (9)C14—C13—C12119.3 (4)
O1—Gd1—C982.72 (10)C14—C13—H13120.4
O4—Gd1—C926.20 (9)C12—C13—H13120.4
O2—Gd1—C994.12 (9)C13—C14—C15119.0 (5)
O6—Gd1—C9124.69 (9)C13—C14—H14120.5
O7—Gd1—C1105.52 (10)C15—C14—H14120.5
O6i—Gd1—C180.75 (9)N2—C15—C14124.1 (4)
O2ii—Gd1—C194.88 (9)N2—C15—H15117.9
O3—Gd1—C176.07 (9)C14—C15—H15117.9
O5—Gd1—C1159.42 (9)N2—C16—C12124.6 (4)
O1—Gd1—C125.62 (10)N2—C16—H16117.7
O4—Gd1—C193.74 (10)C12—C16—H16117.7
O2—Gd1—C126.71 (9)O5—C17—O6119.6 (3)
O6—Gd1—C1147.81 (9)O5—C17—C18120.8 (3)
O7—Gd1—C1774.94 (9)O6—C17—C18119.7 (3)
O6i—Gd1—C1793.45 (9)O5—C17—Gd157.52 (18)
O2ii—Gd1—C1782.75 (9)O6—C17—Gd162.64 (17)
O3—Gd1—C17108.93 (9)C18—C17—Gd1171.9 (3)
O5—Gd1—C1725.77 (9)C19—C18—C17122.8 (3)
O1—Gd1—C17156.00 (9)C19—C18—H18118.6
O4—Gd1—C1792.19 (10)C17—C18—H18118.6
O2—Gd1—C17150.21 (9)C18—C19—C20125.4 (3)
O6—Gd1—C1726.36 (8)C18—C19—H19117.3
C1—O1—Gd195.9 (2)C20—C19—H19117.3
C1—O2—Gd1ii156.8 (2)C21—C20—C24117.4 (4)
C1—O2—Gd191.3 (2)C21—C20—C19120.8 (3)
Gd1ii—O2—Gd1111.81 (8)C24—C20—C19121.8 (3)
C9—O3—Gd194.5 (2)C22—C21—C20119.3 (4)
C9—O4—Gd191.0 (2)C22—C21—H21120.3
C17—O5—Gd196.7 (2)C20—C21—H21120.3
C17—O6—Gd1i156.1 (2)C21—C22—C23119.0 (4)
C17—O6—Gd191.0 (2)C21—C22—H22120.5
Gd1i—O6—Gd1112.91 (9)C23—C22—H22120.5
Gd1—O7—H7A126 (3)N3—C23—C22123.6 (4)
Gd1—O7—H7B116 (3)N3—C23—H23118.2
C7—N1—C8118.2 (4)C22—C23—H23118.2
C15—N2—C16116.0 (4)N3—C24—C20124.3 (4)
C24—N3—C23116.3 (4)N3—C24—H24117.8
O1—C1—O2120.4 (3)C20—C24—H24117.8
O1—C1—C2121.2 (3)
O7—Gd1—O1—C1−162.3 (2)O4—Gd1—C1—O2130.10 (19)
O6i—Gd1—O1—C1−83.6 (2)O6—Gd1—C1—O2−81.3 (2)
O2ii—Gd1—O1—C1−1.6 (2)C9—Gd1—C1—O2104.69 (19)
O3—Gd1—O1—C172.0 (2)O1—C1—C2—C3−4.1 (6)
O5—Gd1—O1—C1133.6 (2)O2—C1—C2—C3176.8 (4)
O4—Gd1—O1—C1125.2 (2)C1—C2—C3—C4176.0 (4)
O2—Gd1—O1—C1−1.9 (2)C2—C3—C4—C8176.6 (4)
O6—Gd1—O1—C1−121.2 (2)C2—C3—C4—C5−6.4 (7)
C9—Gd1—O1—C199.0 (2)C8—C4—C5—C6−0.1 (7)
C17—Gd1—O1—C1−165.9 (2)C3—C4—C5—C6−177.2 (4)
O7—Gd1—O2—C127.5 (2)C4—C5—C6—C71.0 (8)
O6i—Gd1—O2—C191.20 (19)C8—N1—C7—C60.6 (7)
O2ii—Gd1—O2—C1−177.8 (2)C5—C6—C7—N1−1.3 (8)
O3—Gd1—O2—C1−92.5 (2)C7—N1—C8—C40.5 (6)
O5—Gd1—O2—C1−144.5 (2)C5—C4—C8—N1−0.7 (6)
O1—Gd1—O2—C11.87 (19)C3—C4—C8—N1176.6 (4)
O4—Gd1—O2—C1−54.5 (2)Gd1—O4—C9—O312.0 (3)
O6—Gd1—O2—C1130.66 (19)Gd1—O4—C9—C10−166.1 (3)
C9—Gd1—O2—C1−75.6 (2)Gd1—O3—C9—O4−12.5 (4)
C17—Gd1—O2—C1168.76 (19)Gd1—O3—C9—C10165.6 (3)
O7—Gd1—O2—Gd1ii−154.70 (9)O7—Gd1—C9—O4−1.2 (2)
O6i—Gd1—O2—Gd1ii−91.00 (10)O6i—Gd1—C9—O468.4 (4)
O2ii—Gd1—O2—Gd1ii0.0O2ii—Gd1—C9—O4−161.5 (2)
O3—Gd1—O2—Gd1ii85.33 (10)O3—Gd1—C9—O4167.9 (4)
O5—Gd1—O2—Gd1ii33.30 (17)O5—Gd1—C9—O4−85.2 (2)
O1—Gd1—O2—Gd1ii179.67 (14)O1—Gd1—C9—O478.8 (2)
O4—Gd1—O2—Gd1ii123.32 (10)O2—Gd1—C9—O4129.9 (2)
O6—Gd1—O2—Gd1ii−51.55 (14)O6—Gd1—C9—O4−72.0 (2)
C9—Gd1—O2—Gd1ii102.16 (11)C1—Gd1—C9—O4104.1 (2)
C1—Gd1—O2—Gd1ii177.8 (2)C17—Gd1—C9—O4−77.0 (2)
C17—Gd1—O2—Gd1ii−13.4 (2)O7—Gd1—C9—O3−169.1 (2)
O7—Gd1—O3—C913.0 (2)O6i—Gd1—C9—O3−99.5 (4)
O6i—Gd1—O3—C9147.8 (2)O2ii—Gd1—C9—O330.6 (2)
O2ii—Gd1—O3—C9−149.7 (2)O5—Gd1—C9—O3107.0 (2)
O5—Gd1—O3—C9−68.0 (2)O1—Gd1—C9—O3−89.1 (2)
O1—Gd1—O3—C987.5 (2)O4—Gd1—C9—O3−167.9 (4)
O4—Gd1—O3—C96.7 (2)O2—Gd1—C9—O3−37.9 (2)
O2—Gd1—O3—C9140.1 (2)O6—Gd1—C9—O3120.1 (2)
O6—Gd1—O3—C9−81.1 (2)C1—Gd1—C9—O3−63.8 (2)
C1—Gd1—O3—C9112.6 (2)C17—Gd1—C9—O3115.1 (2)
C17—Gd1—O3—C9−71.1 (2)O7—Gd1—C9—C10102.6 (12)
O7—Gd1—O4—C9178.7 (2)O6i—Gd1—C9—C10172.3 (11)
O6i—Gd1—O4—C9−155.2 (2)O2ii—Gd1—C9—C10−57.6 (12)
O2ii—Gd1—O4—C922.9 (3)O3—Gd1—C9—C10−88.3 (13)
O3—Gd1—O4—C9−6.8 (2)O5—Gd1—C9—C1018.7 (12)
O5—Gd1—O4—C987.2 (2)O1—Gd1—C9—C10−177.4 (12)
O1—Gd1—O4—C9−96.9 (2)O4—Gd1—C9—C10103.9 (13)
O2—Gd1—O4—C9−54.6 (2)O2—Gd1—C9—C10−126.2 (12)
O6—Gd1—O4—C9121.5 (2)O6—Gd1—C9—C1031.8 (13)
C1—Gd1—O4—C9−76.1 (2)C1—Gd1—C9—C10−152.0 (12)
C17—Gd1—O4—C9105.5 (2)C17—Gd1—C9—C1026.8 (12)
O7—Gd1—O5—C1762.5 (2)O4—C9—C10—C11179.8 (4)
O6i—Gd1—O5—C17−11.4 (2)O3—C9—C10—C111.7 (6)
O2ii—Gd1—O5—C17−92.5 (2)Gd1—C9—C10—C1182.6 (13)
O3—Gd1—O5—C17−173.1 (2)C9—C10—C11—C12−176.8 (4)
O1—Gd1—O5—C17125.4 (2)C10—C11—C12—C16−173.3 (4)
O4—Gd1—O5—C17134.0 (2)C10—C11—C12—C136.1 (7)
O2—Gd1—O5—C17−123.6 (2)C16—C12—C13—C142.0 (6)
O6—Gd1—O5—C17−5.1 (2)C11—C12—C13—C14−177.4 (4)
C9—Gd1—O5—C17161.2 (2)C12—C13—C14—C15−0.1 (7)
C1—Gd1—O5—C17−171.6 (2)C16—N2—C15—C141.5 (7)
O7—Gd1—O6—C17−96.3 (2)C13—C14—C15—N2−1.8 (8)
O6i—Gd1—O6—C17179.0 (2)C15—N2—C16—C120.6 (7)
O2ii—Gd1—O6—C1789.1 (2)C13—C12—C16—N2−2.4 (6)
O3—Gd1—O6—C1721.6 (2)C11—C12—C16—N2177.0 (4)
O5—Gd1—O6—C174.95 (19)Gd1—O5—C17—O69.2 (4)
O1—Gd1—O6—C17−139.9 (2)Gd1—O5—C17—C18−170.7 (3)
O4—Gd1—O6—C17−38.4 (2)Gd1i—O6—C17—O5168.9 (4)
O2—Gd1—O6—C17136.33 (19)Gd1—O6—C17—O5−8.7 (3)
C9—Gd1—O6—C17−11.2 (2)Gd1i—O6—C17—C18−11.2 (8)
C1—Gd1—O6—C17176.11 (18)Gd1—O6—C17—C18171.2 (3)
O7—Gd1—O6—Gd1i84.78 (11)Gd1i—O6—C17—Gd1177.6 (6)
O6i—Gd1—O6—Gd1i0.0O7—Gd1—C17—O5−113.6 (2)
O2ii—Gd1—O6—Gd1i−89.82 (10)O6i—Gd1—C17—O5170.0 (2)
O3—Gd1—O6—Gd1i−157.36 (9)O2ii—Gd1—C17—O583.7 (2)
O5—Gd1—O6—Gd1i−174.01 (14)O3—Gd1—C17—O57.3 (2)
O1—Gd1—O6—Gd1i41.09 (17)O1—Gd1—C17—O5−110.0 (3)
O4—Gd1—O6—Gd1i142.62 (9)O4—Gd1—C17—O5−43.8 (2)
O2—Gd1—O6—Gd1i−42.63 (14)O2—Gd1—C17—O596.2 (3)
C9—Gd1—O6—Gd1i169.87 (10)O6—Gd1—C17—O5171.0 (3)
C1—Gd1—O6—Gd1i−2.8 (2)C9—Gd1—C17—O5−18.3 (2)
C17—Gd1—O6—Gd1i−179.0 (2)O7—Gd1—C17—O675.42 (19)
Gd1—O1—C1—O23.5 (4)O6i—Gd1—C17—O6−1.0 (2)
Gd1—O1—C1—C2−175.5 (3)O2ii—Gd1—C17—O6−87.35 (19)
Gd1ii—O2—C1—O1−178.2 (4)O3—Gd1—C17—O6−163.73 (18)
Gd1—O2—C1—O1−3.4 (3)O5—Gd1—C17—O6−171.0 (3)
Gd1ii—O2—C1—C20.9 (8)O1—Gd1—C17—O679.0 (3)
Gd1—O2—C1—C2175.7 (3)O4—Gd1—C17—O6145.23 (19)
Gd1ii—O2—C1—Gd1−174.8 (6)O2—Gd1—C17—O6−74.8 (3)
O7—Gd1—C1—O118.1 (2)C9—Gd1—C17—O6170.73 (19)
O6i—Gd1—C1—O192.6 (2)O5—C17—C18—C19−16.9 (6)
O2ii—Gd1—C1—O1178.6 (2)O6—C17—C18—C19163.2 (4)
O3—Gd1—C1—O1−103.3 (2)C17—C18—C19—C20−178.9 (4)
O5—Gd1—C1—O1−104.9 (3)C18—C19—C20—C21153.6 (4)
O4—Gd1—C1—O1−53.3 (2)C18—C19—C20—C24−26.0 (7)
O2—Gd1—C1—O1176.6 (3)C24—C20—C21—C220.5 (7)
O6—Gd1—C1—O195.3 (3)C19—C20—C21—C22−179.1 (4)
C9—Gd1—C1—O1−78.7 (2)C20—C21—C22—C23−0.3 (8)
O7—Gd1—C1—O2−158.44 (18)C24—N3—C23—C220.1 (9)
O6i—Gd1—C1—O2−83.95 (19)C21—C22—C23—N3−0.1 (10)
O2ii—Gd1—C1—O22.1 (2)C23—N3—C24—C200.1 (9)
O3—Gd1—C1—O280.09 (19)C21—C20—C24—N3−0.4 (8)
O5—Gd1—C1—O278.6 (3)C19—C20—C24—N3179.2 (5)
O1—Gd1—C1—O2−176.6 (3)

Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x, −y+1, −z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O7—H7A···N1iii0.853 (10)1.891 (18)2.727 (4)166 (5)
O7—H7B···O3iv0.850 (10)1.908 (13)2.752 (3)172 (4)

Symmetry codes: (iii) −x, −y, −z; (iv) x+1, y, z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: OM2225).

References

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