metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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Bis[μ-2-(4-hydroxyphenyl)acetato]-κ3O,O′:O;κ3O:O,O′-bis­{aqua(4,4′-bi­pyri­dine-κN)bis­[2-(4-hydroxyphenyl)acetato-κ2O,O′]gadolinium(III)} monohydrate

aCollege of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua 321004, People's Republic of China;, Zhejiang Normal University Xingzhi College, Jinhua 321004, People's Republic of China
*Correspondence e-mail: sky53@zjnu.cn

(Received 7 October 2010; accepted 13 October 2010; online 23 October 2010)

In the dinuclear title complex, [Gd2(C8H7O3)6(C10H8N2)2(H2O)2]·H2O, the two GdIII ions are nine-coordinated by seven O atoms from four deprotonated p-hy­droxy­phenyl­acetic acid (PAA) ligands, one water O atom and an N atom from a 4,4′-bypyridine (bipy) ligand in a distorted tricapped trigonal-prismatic geometry. The deprotonated PAA ligands are coordinated to the GdIII atom either as chelating on the same metal or in a tridentate bridging mode. Numerous O—H⋯O and O—H⋯N hydrogen bonds involving hydroxyl, coordinated and uncoordinated water mol­ecules build up an intricate three-dimensional network.

Related literature

For the properties of carb­oxy­lic metal–organic complexes, see: Fang & Zhang (2006[Fang, R.-Q. & Zhang, X.-M. (2006). Inorg. Chem. 45, 4801-4810.]); Liu et al. (2010[Liu, J.-L., Li, H.-Q. & Zhao, G.-L. (2010). Acta Cryst. E66, m9.]); Wang et al. (2010[Wang, G.-H., Lei, Y.-Q. & Wang, N. (2010). Cryst. Growth Des. 10, 4060-4067.]); Wang & Sevov (2008[Wang, X.-X. & Sevov, S. (2008). Inorg. Chem. 47, 1037-1043.]). For related structures, see: Favas et al. (1980[Favas, M. C., Kepert, D. L., Skelton, B. W. & White, A. H. (1980). J. Chem. Soc. Dalton Trans. pp. 454-458.]); Hatscher (2005[Hatscher, S. T. (2005). Private Communication.]); John & Urland (2006[John, D. & Urland, W. (2006). Private Communication.]).

[Scheme 1]

Experimental

Crystal data
  • [Gd2(C8H7O3)6(C10H8N2)2(H2O)2]·H2O

  • Mr = 1587.73

  • Triclinic, [P \overline 1]

  • a = 11.7436 (1) Å

  • b = 16.2654 (2) Å

  • c = 18.4311 (2) Å

  • α = 83.52 (1)°

  • β = 72.11 (1)°

  • γ = 71.10 (1)°

  • V = 3169.4 (3) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 2.16 mm−1

  • T = 296 K

  • 0.15 × 0.13 × 0.12 mm

Data collection
  • Bruker APEXII area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.731, Tmax = 0.772

  • 41430 measured reflections

  • 11119 independent reflections

  • 9631 reflections with I > 2σ(I)

  • Rint = 0.026

Refinement
  • R[F2 > 2σ(F2)] = 0.020

  • wR(F2) = 0.048

  • S = 1.05

  • 11117 reflections

  • 862 parameters

  • H-atom parameters constrained

  • Δρmax = 0.45 e Å−3

  • Δρmin = −0.43 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O1W—H1WB⋯O13 0.77 2.00 2.744 (2) 161
O1W—H1WA⋯N4i 0.78 2.02 2.784 (3) 167
O2W—H2WB⋯O1 0.82 2.00 2.750 (2) 151
O2W—H2WA⋯N2ii 0.83 2.03 2.842 (3) 167
O3—H3⋯O3W 0.82 1.86 2.641 (3) 160
O6—H6⋯O12i 0.82 1.94 2.743 (3) 168
O9—H9⋯O17iii 0.82 1.87 2.675 (3) 167
O12—H12⋯O11iv 0.82 1.94 2.750 (3) 167
O15—H15⋯O3v 0.82 1.90 2.717 (3) 174
O18—H18⋯O9ii 0.82 1.97 2.767 (3) 162
O3W—H3WA⋯O4vi 0.81 1.96 2.773 (3) 179
O3W—H3WB⋯O6ii 0.83 1.99 2.808 (3) 165
Symmetry codes: (i) x, y-1, z; (ii) x, y+1, z; (iii) -x+2, -y, -z+1; (iv) -x+2, -y+1, -z; (v) x+1, y-1, z; (vi) -x+1, -y+1, -z.

Data collection: APEX2 (Bruker, 2006[Bruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2006[Bruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEPIII (Burnett & Johnson, 1996[Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.]) and ORTEP-3 for Windows (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

The design and synthesis of carboxylic metal-organic complexes have attracted increasing interest for decades owing to their potential practical applications, such as fluorescence, magnetism (Wang, et al., 2010; Fang, et al., 2006; Wang, et al., 2008). As part of our interest in this field (Liu, et al., 2010), we report here the crystal structure of a new gadolinium(III) complex with the ligand p-hydroxyphenylacetic acid.

In the dinuclear title complex, the two GdIII ions are nine coordinated by four p-hydroxyphenylacetic acid(PAA) ligands via seven O atoms, one O atom from water molecule and a N atom from bipy ligand in a distorted tricapped trigonal-prismatic geometry. Futhermore, the asymmetric unit contains one solvent water molecules (Fig. 1). Bond lengths and bond angles involving the metals and O atoms skeleton compare well with related structure as bis((µ2-Acetato-O,O,O')-diaqua-bis(acetato-O,O')-gadolinium(iii)) tetrahydrate (Favas et al., 1980), bis(µ2-Acetato-O,O,O')-tetrakis(acetato-O,O')-tetra-aqua-di-gadolinium tetrahydrate (Hatscher, 2005) or bis(\m2-Acetato)-tetrakis(acetato)-diaqua-bis(4-pyridyloxy)-di-gadolinium dihydrate (John & Urland, 2006).

Numerous O-H···O hydrogen bonds involving hydroxyl, coordinated and non-coordinated water molecules, build up an intricated three dimensionnal network (Table 1).

Related literature top

For the properties of carboxylic metal–organic complexes, see: Fang & Zhang (2006); Liu et al. (2010); Wang et al. (2010); Wang & Sevov (2008). For related structures, see: Favas et al. (1980); Hatscher (2005); John & Urland (2006).

Experimental top

All reagents and solvents were of commercially available quality and were used without further purification. P-hydroxyphenylacetic acid(HPAA)(3mmol) and sodium hydroxide (3mmol) were mixed together in water(10ml), then Gd[(NO3)3](1mmol) dissolved in water(10ml) was added into the above solution. After stirring for one hour, an ethanol(5ml) solution of 4,4'-bipyridine(1 mmol) was slowly dropped into the above solution with stirring for three hours. After filtration, the filtrate was allowed to stand at room temperature, and single crystals suitable for X-ray work were obtained after a week.

Refinement top

All H atoms attached to C atoms and O(hydroxyl) atom were fixed geometrically and treated as riding with C—H = 0.97 Å (methylene) or 0.93 Å (aromatic) and O—H = 0.82 Å with Uiso(H) = 1.2Ueq(C) or Uiso(H) = 1.5Ueq(O). H atoms of water molecule were located in a difference Fourier map and included in the subsequent refinement using restraints (O-H= 0.82 (1)Å and H···H= 1.39 (2)Å) with Uiso(H) = 1.5Ueq(O). In the last cycles of refinement they were treated as riding on their parent O atom.

Structure description top

The design and synthesis of carboxylic metal-organic complexes have attracted increasing interest for decades owing to their potential practical applications, such as fluorescence, magnetism (Wang, et al., 2010; Fang, et al., 2006; Wang, et al., 2008). As part of our interest in this field (Liu, et al., 2010), we report here the crystal structure of a new gadolinium(III) complex with the ligand p-hydroxyphenylacetic acid.

In the dinuclear title complex, the two GdIII ions are nine coordinated by four p-hydroxyphenylacetic acid(PAA) ligands via seven O atoms, one O atom from water molecule and a N atom from bipy ligand in a distorted tricapped trigonal-prismatic geometry. Futhermore, the asymmetric unit contains one solvent water molecules (Fig. 1). Bond lengths and bond angles involving the metals and O atoms skeleton compare well with related structure as bis((µ2-Acetato-O,O,O')-diaqua-bis(acetato-O,O')-gadolinium(iii)) tetrahydrate (Favas et al., 1980), bis(µ2-Acetato-O,O,O')-tetrakis(acetato-O,O')-tetra-aqua-di-gadolinium tetrahydrate (Hatscher, 2005) or bis(\m2-Acetato)-tetrakis(acetato)-diaqua-bis(4-pyridyloxy)-di-gadolinium dihydrate (John & Urland, 2006).

Numerous O-H···O hydrogen bonds involving hydroxyl, coordinated and non-coordinated water molecules, build up an intricated three dimensionnal network (Table 1).

For the properties of carboxylic metal–organic complexes, see: Fang & Zhang (2006); Liu et al. (2010); Wang et al. (2010); Wang & Sevov (2008). For related structures, see: Favas et al. (1980); Hatscher (2005); John & Urland (2006).

Computing details top

Data collection: APEX2 (Bruker, 2006); cell refinement: SAINT (Bruker, 2006); data reduction: SAINT (Bruker, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title complex, showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omited for the sake of clarity.
Bis[µ-2-(4-hydroxyphenyl)acetato]- κ3O,O':O;κ3O:O,O'- bis{aqua(4,4'-bipyridine-κN)bis[2-(4-hydroxyphenyl)acetato- κ2O,O']gadolinium(III)} monohydrate top
Crystal data top
[Gd2(C8H7O3)6(C10H8N2)2(H2O)2]·H2OZ = 2
Mr = 1587.73F(000) = 1592
Triclinic, P1Dx = 1.664 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.7436 (1) ÅCell parameters from 9500 reflections
b = 16.2654 (2) Åθ = 1.2–25.0°
c = 18.4311 (2) ŵ = 2.16 mm1
α = 83.52 (1)°T = 296 K
β = 72.11 (1)°Block, colourless
γ = 71.10 (1)°0.15 × 0.13 × 0.12 mm
V = 3169.4 (3) Å3
Data collection top
Bruker APEXII area-detector
diffractometer
11119 independent reflections
Radiation source: fine-focus sealed tube9631 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
φ and ω scansθmax = 25.0°, θmin = 1.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1313
Tmin = 0.731, Tmax = 0.772k = 1918
41430 measured reflectionsl = 2121
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) = 0.048H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0216P)2 + 0.9907P]
where P = (Fo2 + 2Fc2)/3
11117 reflections(Δ/σ)max = 0.003
862 parametersΔρmax = 0.45 e Å3
0 restraintsΔρmin = 0.43 e Å3
Crystal data top
[Gd2(C8H7O3)6(C10H8N2)2(H2O)2]·H2Oγ = 71.10 (1)°
Mr = 1587.73V = 3169.4 (3) Å3
Triclinic, P1Z = 2
a = 11.7436 (1) ÅMo Kα radiation
b = 16.2654 (2) ŵ = 2.16 mm1
c = 18.4311 (2) ÅT = 296 K
α = 83.52 (1)°0.15 × 0.13 × 0.12 mm
β = 72.11 (1)°
Data collection top
Bruker APEXII area-detector
diffractometer
11119 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
9631 reflections with I > 2σ(I)
Tmin = 0.731, Tmax = 0.772Rint = 0.026
41430 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0200 restraints
wR(F2) = 0.048H-atom parameters constrained
S = 1.05Δρmax = 0.45 e Å3
11117 reflectionsΔρmin = 0.43 e Å3
862 parameters
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Gd10.728426 (10)0.135737 (7)0.216706 (6)0.02445 (4)
Gd20.868375 (10)0.292972 (7)0.303667 (6)0.02434 (4)
O10.58635 (16)0.28209 (10)0.22392 (11)0.0379 (4)
O1W0.91582 (16)0.04089 (10)0.24569 (10)0.0384 (4)
H1WA0.94210.00950.24890.058*
H1WB0.95580.06060.26060.058*
O20.50408 (16)0.17705 (11)0.23605 (11)0.0440 (5)
O2W0.67324 (16)0.38841 (10)0.28455 (10)0.0389 (4)
H2WA0.64230.44190.28800.058*
H2WB0.62630.37290.26800.058*
O30.3780 (2)0.66676 (12)0.14719 (11)0.0576 (6)
H30.39720.67610.10100.086*
O40.69157 (18)0.16439 (12)0.08673 (10)0.0437 (5)
O50.86409 (16)0.06658 (11)0.09667 (10)0.0381 (4)
O60.6696 (2)0.23208 (13)0.01187 (15)0.0639 (6)
H60.72740.26990.03850.096*
O70.64767 (18)0.10012 (12)0.35152 (10)0.0448 (5)
O80.74284 (15)0.19881 (10)0.33397 (9)0.0302 (4)
O90.83523 (19)0.21253 (12)0.55882 (13)0.0544 (5)
H90.90980.22930.55720.082*
O100.85702 (15)0.23143 (10)0.18638 (9)0.0295 (4)
O110.91748 (17)0.34765 (11)0.16459 (10)0.0363 (4)
O120.85826 (18)0.62580 (11)0.08206 (11)0.0460 (5)
H120.93020.62660.10360.069*
O131.01650 (15)0.14806 (10)0.29342 (11)0.0376 (4)
O141.09358 (16)0.25591 (10)0.25472 (11)0.0414 (5)
O151.2910 (2)0.24392 (11)0.27918 (11)0.0532 (5)
H151.31720.26720.23750.080*
O160.73943 (16)0.34546 (11)0.43136 (10)0.0391 (4)
O170.93402 (18)0.27265 (12)0.42362 (10)0.0461 (5)
O180.6549 (2)0.71630 (13)0.55102 (16)0.0720 (7)
H180.70510.73340.56290.108*
N10.68739 (19)0.01014 (13)0.21714 (12)0.0332 (5)
N20.6042 (3)0.42714 (17)0.2815 (2)0.0662 (8)
N30.91443 (19)0.43674 (12)0.31052 (11)0.0319 (5)
N40.9696 (3)0.86188 (16)0.2689 (2)0.0654 (8)
C10.3770 (2)0.41132 (16)0.19719 (16)0.0366 (6)
C20.3614 (3)0.46773 (17)0.25268 (16)0.0422 (7)
H2A0.34990.44830.30310.051*
C30.3625 (3)0.55184 (17)0.23510 (15)0.0432 (7)
H3B0.35160.58860.27340.052*
C40.3796 (2)0.58167 (16)0.16114 (15)0.0370 (6)
C50.3960 (3)0.52712 (18)0.10483 (16)0.0483 (7)
H5A0.40720.54700.05460.058*
C60.3957 (3)0.44209 (17)0.12320 (17)0.0488 (7)
H6B0.40850.40500.08460.059*
C70.3744 (3)0.31993 (17)0.21737 (19)0.0482 (7)
H7A0.35230.29900.17790.058*
H7B0.30810.32090.26450.058*
C80.4950 (2)0.25578 (16)0.22693 (14)0.0335 (6)
C90.7748 (2)0.01008 (16)0.01699 (14)0.0348 (6)
C100.8552 (2)0.08123 (18)0.06146 (16)0.0428 (7)
H10A0.93380.07940.09200.051*
C110.8202 (3)0.15419 (18)0.06094 (17)0.0463 (7)
H11A0.87420.20060.09210.056*
C120.7060 (3)0.15891 (18)0.01472 (16)0.0429 (7)
C130.6246 (3)0.08902 (19)0.02885 (17)0.0493 (7)
H13A0.54630.09140.05940.059*
C140.6589 (3)0.01520 (18)0.02744 (16)0.0437 (7)
H14A0.60290.03190.05700.052*
C150.8144 (3)0.07057 (17)0.02025 (14)0.0404 (6)
H15B0.90350.05730.04650.048*
H15C0.76910.11590.04910.048*
C160.7889 (2)0.10286 (16)0.05820 (14)0.0333 (6)
C170.7278 (3)0.04549 (17)0.48684 (14)0.0411 (7)
C180.8537 (3)0.0015 (2)0.47187 (15)0.0470 (7)
H18B0.91400.02520.44570.056*
C190.8920 (3)0.08767 (19)0.49510 (15)0.0434 (7)
H19A0.97720.11830.48440.052*
C200.8035 (3)0.12784 (17)0.53414 (15)0.0388 (6)
C210.6774 (3)0.08183 (17)0.54898 (15)0.0403 (6)
H21A0.61710.10870.57490.048*
C220.6406 (3)0.00349 (17)0.52551 (15)0.0415 (7)
H22A0.55530.03360.53580.050*
C230.6874 (4)0.13873 (18)0.46056 (16)0.0563 (9)
H23A0.74200.16850.46840.068*
H23B0.60240.16730.49100.068*
C240.6918 (2)0.14594 (15)0.37741 (14)0.0312 (6)
C250.8584 (3)0.38624 (17)0.02357 (15)0.0382 (6)
C260.9606 (3)0.39378 (18)0.03605 (15)0.0421 (7)
H26A1.02960.34480.05190.051*
C270.9619 (3)0.47269 (18)0.07246 (15)0.0410 (7)
H27A1.03060.47650.11300.049*
C280.8612 (2)0.54537 (16)0.04844 (14)0.0352 (6)
C290.7580 (3)0.53954 (18)0.01059 (15)0.0414 (7)
H29A0.68940.58870.02650.050*
C300.7572 (3)0.46032 (18)0.04574 (15)0.0422 (7)
H30A0.68720.45650.08520.051*
C310.8567 (3)0.30136 (17)0.06579 (15)0.0439 (7)
H31A0.77590.29310.07240.053*
H31B0.92060.25440.03450.053*
C320.8789 (2)0.29443 (15)0.14252 (14)0.0295 (5)
C331.2555 (2)0.01976 (15)0.25513 (14)0.0312 (6)
C341.3105 (2)0.03315 (16)0.19210 (15)0.0367 (6)
H34A1.33960.00920.14440.044*
C351.3233 (3)0.12107 (17)0.19864 (15)0.0407 (7)
H35A1.36020.15550.15550.049*
C361.2812 (2)0.15756 (16)0.26898 (15)0.0365 (6)
C371.2250 (3)0.10546 (17)0.33231 (15)0.0395 (6)
H37A1.19540.12940.37990.047*
C381.2129 (2)0.01870 (16)0.32502 (15)0.0375 (6)
H38A1.17510.01560.36820.045*
C391.2429 (2)0.11494 (15)0.24847 (16)0.0365 (6)
H39A1.28820.12720.19690.044*
H39B1.28350.12750.28260.044*
C401.1101 (2)0.17600 (15)0.26615 (14)0.0301 (6)
C410.7657 (3)0.44631 (17)0.54653 (14)0.0377 (6)
C420.8463 (3)0.48886 (19)0.55337 (15)0.0444 (7)
H42A0.92590.45630.55680.053*
C430.8120 (3)0.57845 (19)0.55530 (17)0.0500 (7)
H43A0.86820.60550.55970.060*
C440.6939 (3)0.62779 (18)0.55074 (16)0.0455 (7)
C450.6105 (3)0.58671 (18)0.54578 (15)0.0442 (7)
H45A0.53000.61930.54420.053*
C460.6470 (3)0.49732 (17)0.54315 (15)0.0406 (6)
H46A0.59050.47040.53900.049*
C470.8076 (3)0.34842 (17)0.54043 (15)0.0450 (7)
H47A0.88520.32400.55440.054*
H47B0.74440.32580.57610.054*
C480.8279 (3)0.32041 (15)0.46111 (14)0.0346 (6)
C490.5820 (2)0.02120 (16)0.26501 (16)0.0395 (6)
H49A0.52180.02670.29180.047*
C500.5573 (3)0.09981 (16)0.27694 (17)0.0443 (7)
H50A0.48270.10430.31140.053*
C510.6443 (2)0.17179 (16)0.23729 (15)0.0365 (6)
C520.7519 (3)0.16002 (16)0.18590 (15)0.0380 (6)
H52A0.81190.20630.15690.046*
C530.7699 (2)0.07956 (16)0.17772 (15)0.0371 (6)
H53A0.84320.07320.14300.045*
C540.5497 (3)0.3656 (2)0.3339 (2)0.0725 (11)
H54A0.50260.37940.38150.087*
C550.5587 (3)0.28205 (19)0.3216 (2)0.0603 (9)
H55A0.51980.24180.36060.072*
C560.6260 (3)0.25908 (17)0.25117 (17)0.0423 (7)
C570.6791 (4)0.3219 (2)0.1960 (2)0.0622 (9)
H57A0.72330.30930.14700.075*
C580.6661 (4)0.4037 (2)0.2141 (2)0.0721 (11)
H58A0.70370.44520.17610.086*
C590.8281 (3)0.50330 (16)0.35255 (15)0.0382 (6)
H59A0.75500.49420.38510.046*
C600.8423 (3)0.58449 (16)0.34988 (15)0.0412 (7)
H60A0.77990.62830.38070.049*
C610.9487 (3)0.60137 (15)0.30181 (15)0.0359 (6)
C621.0403 (3)0.53139 (16)0.26052 (16)0.0410 (7)
H62A1.11530.53830.22860.049*
C631.0199 (2)0.45177 (16)0.26701 (15)0.0375 (6)
H63A1.08340.40580.23940.045*
C640.8901 (4)0.8392 (2)0.3297 (2)0.0704 (11)
H64A0.83600.88200.36460.084*
C650.8832 (4)0.75557 (19)0.34439 (18)0.0624 (10)
H65A0.82720.74280.38880.075*
C660.9601 (3)0.69054 (17)0.29244 (17)0.0426 (7)
C671.0436 (3)0.71389 (19)0.2294 (2)0.0600 (9)
H67A1.09810.67280.19310.072*
C681.0455 (3)0.7992 (2)0.2207 (3)0.0719 (11)
H68A1.10390.81330.17830.086*
O3W0.44251 (19)0.73311 (13)0.00868 (11)0.0560 (5)
H3WA0.40280.76300.01890.084*
H3WB0.50180.75300.00310.084*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Gd10.02817 (7)0.01682 (6)0.03181 (7)0.00953 (5)0.01159 (5)0.00229 (5)
Gd20.02690 (7)0.01577 (6)0.03249 (7)0.00774 (5)0.01046 (5)0.00023 (5)
O10.0336 (10)0.0231 (9)0.0645 (12)0.0083 (8)0.0242 (9)0.0037 (8)
O1W0.0424 (10)0.0189 (9)0.0616 (12)0.0085 (8)0.0274 (9)0.0009 (8)
O20.0350 (10)0.0226 (10)0.0765 (14)0.0115 (8)0.0193 (9)0.0091 (9)
O2W0.0386 (10)0.0203 (9)0.0631 (12)0.0061 (7)0.0244 (9)0.0025 (8)
O30.0959 (17)0.0309 (11)0.0457 (12)0.0269 (11)0.0122 (12)0.0002 (9)
O40.0525 (12)0.0358 (11)0.0412 (11)0.0047 (9)0.0190 (9)0.0054 (8)
O50.0381 (10)0.0423 (11)0.0365 (10)0.0152 (8)0.0113 (8)0.0005 (8)
O60.0513 (13)0.0441 (13)0.0957 (18)0.0242 (11)0.0054 (12)0.0141 (12)
O70.0649 (13)0.0493 (12)0.0372 (11)0.0414 (10)0.0154 (10)0.0057 (9)
O80.0354 (9)0.0214 (9)0.0364 (10)0.0145 (7)0.0092 (8)0.0040 (7)
O90.0582 (13)0.0342 (11)0.0807 (15)0.0142 (10)0.0373 (12)0.0093 (10)
O100.0334 (9)0.0219 (9)0.0359 (10)0.0138 (7)0.0103 (8)0.0059 (7)
O110.0501 (11)0.0329 (10)0.0377 (10)0.0269 (9)0.0169 (9)0.0076 (8)
O120.0506 (12)0.0326 (10)0.0544 (13)0.0190 (9)0.0123 (10)0.0119 (9)
O130.0296 (9)0.0227 (9)0.0629 (12)0.0093 (7)0.0144 (9)0.0033 (8)
O140.0349 (10)0.0184 (9)0.0654 (13)0.0068 (7)0.0093 (9)0.0020 (8)
O150.0790 (15)0.0256 (10)0.0578 (13)0.0170 (10)0.0224 (12)0.0010 (9)
O160.0402 (10)0.0376 (11)0.0429 (11)0.0151 (8)0.0119 (9)0.0041 (8)
O170.0501 (12)0.0410 (11)0.0415 (11)0.0015 (9)0.0188 (9)0.0087 (9)
O180.0797 (17)0.0332 (12)0.110 (2)0.0202 (11)0.0326 (15)0.0031 (12)
N10.0345 (12)0.0240 (11)0.0449 (13)0.0125 (9)0.0135 (10)0.0008 (9)
N20.0628 (18)0.0322 (15)0.119 (3)0.0242 (14)0.0441 (18)0.0163 (16)
N30.0404 (12)0.0225 (11)0.0359 (12)0.0108 (9)0.0141 (10)0.0007 (9)
N40.082 (2)0.0296 (15)0.115 (3)0.0256 (15)0.068 (2)0.0154 (16)
C10.0265 (13)0.0261 (14)0.0595 (18)0.0045 (11)0.0196 (13)0.0001 (12)
C20.0502 (17)0.0346 (15)0.0404 (16)0.0118 (13)0.0138 (13)0.0040 (12)
C30.0596 (19)0.0320 (15)0.0388 (16)0.0130 (13)0.0139 (14)0.0069 (12)
C40.0439 (15)0.0256 (14)0.0398 (16)0.0086 (11)0.0113 (12)0.0017 (11)
C50.068 (2)0.0371 (16)0.0367 (16)0.0113 (14)0.0153 (14)0.0021 (12)
C60.065 (2)0.0297 (15)0.0522 (18)0.0034 (14)0.0261 (15)0.0110 (13)
C70.0398 (16)0.0291 (15)0.081 (2)0.0091 (12)0.0272 (15)0.0040 (14)
C80.0334 (14)0.0294 (15)0.0383 (15)0.0084 (11)0.0128 (12)0.0011 (11)
C90.0411 (15)0.0362 (15)0.0317 (14)0.0150 (12)0.0131 (12)0.0012 (11)
C100.0325 (15)0.0439 (17)0.0487 (17)0.0144 (13)0.0010 (13)0.0097 (13)
C110.0381 (16)0.0387 (16)0.0575 (19)0.0099 (13)0.0042 (14)0.0150 (13)
C120.0393 (16)0.0401 (16)0.0534 (18)0.0148 (13)0.0153 (14)0.0033 (13)
C130.0348 (15)0.0531 (19)0.0560 (19)0.0168 (14)0.0013 (14)0.0076 (15)
C140.0398 (16)0.0415 (16)0.0450 (17)0.0098 (13)0.0033 (13)0.0139 (13)
C150.0507 (17)0.0399 (16)0.0325 (15)0.0184 (13)0.0099 (13)0.0001 (12)
C160.0412 (15)0.0291 (14)0.0343 (14)0.0212 (12)0.0074 (12)0.0026 (11)
C170.069 (2)0.0378 (16)0.0287 (14)0.0284 (15)0.0196 (14)0.0038 (11)
C180.062 (2)0.060 (2)0.0336 (16)0.0424 (17)0.0117 (14)0.0041 (13)
C190.0433 (16)0.0516 (18)0.0402 (16)0.0202 (14)0.0107 (13)0.0071 (13)
C200.0488 (17)0.0343 (15)0.0417 (16)0.0165 (13)0.0213 (13)0.0002 (12)
C210.0439 (16)0.0361 (15)0.0489 (17)0.0237 (13)0.0157 (13)0.0082 (12)
C220.0502 (17)0.0362 (16)0.0436 (16)0.0159 (13)0.0200 (14)0.0041 (12)
C230.109 (3)0.0388 (17)0.0372 (17)0.0405 (18)0.0273 (17)0.0083 (13)
C240.0378 (14)0.0246 (13)0.0325 (14)0.0123 (11)0.0104 (11)0.0031 (10)
C250.0566 (18)0.0360 (15)0.0346 (15)0.0250 (13)0.0228 (13)0.0093 (11)
C260.0521 (17)0.0346 (15)0.0397 (16)0.0127 (13)0.0142 (14)0.0005 (12)
C270.0444 (16)0.0420 (16)0.0362 (15)0.0176 (13)0.0084 (13)0.0045 (12)
C280.0433 (15)0.0333 (15)0.0380 (15)0.0204 (12)0.0182 (13)0.0085 (11)
C290.0414 (16)0.0382 (16)0.0441 (16)0.0134 (13)0.0121 (13)0.0043 (12)
C300.0468 (17)0.0464 (17)0.0372 (16)0.0250 (14)0.0096 (13)0.0090 (13)
C310.068 (2)0.0359 (16)0.0426 (16)0.0304 (14)0.0257 (15)0.0105 (12)
C320.0316 (13)0.0232 (13)0.0350 (14)0.0114 (10)0.0098 (11)0.0037 (10)
C330.0258 (13)0.0257 (13)0.0409 (15)0.0039 (10)0.0114 (11)0.0026 (11)
C340.0395 (15)0.0301 (14)0.0337 (14)0.0052 (11)0.0073 (12)0.0009 (11)
C350.0481 (16)0.0317 (15)0.0382 (16)0.0034 (12)0.0122 (13)0.0109 (12)
C360.0435 (15)0.0237 (13)0.0461 (16)0.0096 (11)0.0189 (13)0.0010 (11)
C370.0460 (16)0.0355 (15)0.0353 (15)0.0138 (12)0.0082 (12)0.0001 (12)
C380.0401 (15)0.0293 (14)0.0378 (15)0.0040 (12)0.0077 (12)0.0096 (11)
C390.0317 (14)0.0261 (13)0.0514 (17)0.0079 (11)0.0115 (12)0.0031 (11)
C400.0305 (13)0.0251 (14)0.0361 (14)0.0069 (11)0.0114 (11)0.0059 (10)
C410.0509 (17)0.0361 (15)0.0273 (14)0.0162 (13)0.0087 (12)0.0030 (11)
C420.0412 (16)0.0470 (18)0.0437 (17)0.0103 (13)0.0106 (13)0.0092 (13)
C430.0513 (18)0.0504 (19)0.0537 (19)0.0260 (15)0.0095 (15)0.0067 (14)
C440.0556 (18)0.0344 (16)0.0458 (17)0.0177 (14)0.0086 (14)0.0032 (12)
C450.0457 (16)0.0397 (17)0.0453 (17)0.0123 (13)0.0121 (13)0.0014 (13)
C460.0446 (16)0.0419 (17)0.0377 (15)0.0182 (13)0.0098 (13)0.0009 (12)
C470.0660 (19)0.0344 (16)0.0335 (15)0.0129 (14)0.0160 (14)0.0017 (12)
C480.0495 (17)0.0208 (13)0.0353 (15)0.0143 (12)0.0124 (13)0.0035 (11)
C490.0351 (15)0.0234 (14)0.0586 (18)0.0089 (11)0.0104 (13)0.0044 (12)
C500.0348 (15)0.0276 (15)0.070 (2)0.0137 (12)0.0124 (14)0.0053 (13)
C510.0424 (15)0.0235 (13)0.0523 (17)0.0134 (12)0.0242 (13)0.0049 (11)
C520.0443 (16)0.0233 (13)0.0466 (16)0.0095 (12)0.0131 (13)0.0035 (11)
C530.0388 (15)0.0291 (14)0.0453 (16)0.0131 (12)0.0124 (13)0.0017 (12)
C540.050 (2)0.041 (2)0.116 (3)0.0193 (16)0.013 (2)0.024 (2)
C550.0447 (18)0.0318 (16)0.091 (3)0.0124 (14)0.0016 (17)0.0048 (16)
C560.0428 (16)0.0289 (15)0.066 (2)0.0168 (12)0.0275 (15)0.0083 (13)
C570.099 (3)0.0400 (18)0.064 (2)0.0371 (18)0.032 (2)0.0025 (15)
C580.113 (3)0.0343 (18)0.093 (3)0.031 (2)0.053 (3)0.0005 (18)
C590.0455 (16)0.0277 (14)0.0398 (15)0.0141 (12)0.0083 (13)0.0033 (11)
C600.0549 (18)0.0227 (14)0.0429 (16)0.0082 (12)0.0130 (14)0.0026 (11)
C610.0500 (16)0.0233 (13)0.0458 (16)0.0148 (12)0.0285 (14)0.0066 (11)
C620.0390 (15)0.0297 (15)0.0590 (18)0.0159 (12)0.0168 (14)0.0047 (13)
C630.0378 (15)0.0260 (14)0.0496 (17)0.0122 (11)0.0108 (13)0.0017 (11)
C640.129 (3)0.0304 (17)0.074 (2)0.025 (2)0.061 (2)0.0011 (16)
C650.118 (3)0.0331 (17)0.054 (2)0.0319 (18)0.043 (2)0.0039 (14)
C660.0564 (18)0.0263 (14)0.0613 (19)0.0184 (13)0.0364 (15)0.0082 (13)
C670.0455 (18)0.0339 (17)0.103 (3)0.0163 (14)0.0243 (18)0.0114 (17)
C680.051 (2)0.040 (2)0.133 (3)0.0240 (16)0.037 (2)0.027 (2)
O3W0.0613 (13)0.0543 (13)0.0596 (13)0.0247 (11)0.0270 (11)0.0189 (10)
Geometric parameters (Å, º) top
Gd1—O102.4132 (15)C17—C231.506 (4)
Gd1—O12.4146 (16)C18—C191.387 (4)
Gd1—O1W2.4177 (16)C18—H18B0.9300
Gd1—O22.4187 (17)C19—C201.379 (4)
Gd1—O52.4359 (17)C19—H19A0.9300
Gd1—O72.4480 (17)C20—C211.381 (4)
Gd1—O42.5295 (18)C21—C221.375 (4)
Gd1—O82.5671 (16)C21—H21A0.9300
Gd1—N12.568 (2)C22—H22A0.9300
Gd1—C82.768 (2)C23—C241.510 (4)
Gd1—C162.856 (3)C23—H23A0.9700
Gd1—C242.875 (2)C23—H23B0.9700
Gd2—O82.3653 (15)C25—C301.384 (4)
Gd2—O142.4075 (17)C25—C261.385 (4)
Gd2—O2W2.4193 (16)C25—C311.509 (3)
Gd2—O132.4207 (16)C26—C271.382 (4)
Gd2—O162.4469 (18)C26—H26A0.9300
Gd2—O172.5118 (18)C27—C281.372 (4)
Gd2—O102.5387 (16)C27—H27A0.9300
Gd2—O112.5697 (16)C28—C291.380 (4)
Gd2—N32.5893 (19)C29—C301.377 (4)
Gd2—C402.784 (2)C29—H29A0.9300
Gd2—C482.855 (3)C30—H30A0.9300
Gd2—C322.932 (2)C31—C321.501 (3)
O1—C81.262 (3)C31—H31A0.9700
O1W—H1WA0.7792C31—H31B0.9700
O1W—H1WB0.7713C33—C341.383 (3)
O2—C81.246 (3)C33—C381.388 (3)
O2W—H2WA0.8281C33—C391.501 (3)
O2W—H2WB0.8199C34—C351.384 (4)
O3—C41.374 (3)C34—H34A0.9300
O3—H30.8200C35—C361.378 (4)
O4—C161.262 (3)C35—H35A0.9300
O5—C161.258 (3)C36—C371.380 (4)
O6—C121.379 (3)C37—C381.367 (4)
O6—H60.8200C37—H37A0.9300
O7—C241.238 (3)C38—H38A0.9300
O8—C241.275 (3)C39—C401.510 (3)
O9—C201.369 (3)C39—H39A0.9700
O9—H90.8200C39—H39B0.9700
O10—C321.275 (3)C41—C421.381 (4)
O11—C321.252 (3)C41—C461.389 (4)
O12—C281.377 (3)C41—C471.513 (4)
O12—H120.8200C42—C431.382 (4)
O13—C401.265 (3)C42—H42A0.9300
O14—C401.254 (3)C43—C441.382 (4)
O15—C361.368 (3)C43—H43A0.9300
O15—H150.8200C44—C451.381 (4)
O16—C481.253 (3)C45—C461.378 (4)
O17—C481.265 (3)C45—H45A0.9300
O18—C441.362 (3)C46—H46A0.9300
O18—H180.8200C47—C481.506 (4)
N1—C491.335 (3)C47—H47A0.9700
N1—C531.336 (3)C47—H47B0.9700
N2—C581.316 (5)C49—C501.380 (3)
N2—C541.329 (5)C49—H49A0.9300
N3—C631.333 (3)C50—C511.382 (4)
N3—C591.340 (3)C50—H50A0.9300
N4—C641.323 (5)C51—C521.382 (4)
N4—C681.324 (5)C51—C561.487 (3)
C1—C61.375 (4)C52—C531.377 (3)
C1—C21.382 (4)C52—H52A0.9300
C1—C71.499 (4)C53—H53A0.9300
C2—C31.373 (4)C54—C551.385 (4)
C2—H2A0.9300C54—H54A0.9300
C3—C41.371 (4)C55—C561.379 (4)
C3—H3B0.9300C55—H55A0.9300
C4—C51.370 (4)C56—C571.378 (4)
C5—C61.387 (4)C57—C581.381 (4)
C5—H5A0.9300C57—H57A0.9300
C6—H6B0.9300C58—H58A0.9300
C7—C81.510 (3)C59—C601.378 (4)
C7—H7A0.9700C59—H59A0.9300
C7—H7B0.9700C60—C611.381 (4)
C9—C141.379 (4)C60—H60A0.9300
C9—C101.391 (4)C61—C621.390 (4)
C9—C151.517 (4)C61—C661.485 (3)
C10—C111.374 (4)C62—C631.378 (3)
C10—H10A0.9300C62—H62A0.9300
C11—C121.372 (4)C63—H63A0.9300
C11—H11A0.9300C64—C651.381 (4)
C12—C131.371 (4)C64—H64A0.9300
C13—C141.380 (4)C65—C661.389 (4)
C13—H13A0.9300C65—H65A0.9300
C14—H14A0.9300C66—C671.377 (4)
C15—C161.503 (3)C67—C681.385 (4)
C15—H15B0.9700C67—H67A0.9300
C15—H15C0.9700C68—H68A0.9300
C17—C181.383 (4)O3W—H3WA0.8095
C17—C221.385 (4)O3W—H3WB0.8339
O10—Gd1—O173.49 (5)C12—C11—H11A119.9
O10—Gd1—O1W79.74 (5)C10—C11—H11A119.9
O1—Gd1—O1W145.42 (6)C13—C12—C11119.6 (3)
O10—Gd1—O2126.77 (5)C13—C12—O6118.9 (3)
O1—Gd1—O253.62 (6)C11—C12—O6121.5 (3)
O1W—Gd1—O2149.95 (6)C12—C13—C14120.1 (3)
O10—Gd1—O584.86 (6)C12—C13—H13A120.0
O1—Gd1—O5123.03 (6)C14—C13—H13A120.0
O1W—Gd1—O574.79 (6)C9—C14—C13121.2 (3)
O2—Gd1—O5117.09 (6)C9—C14—H14A119.4
O10—Gd1—O7117.15 (6)C13—C14—H14A119.4
O1—Gd1—O795.22 (7)C16—C15—C9111.5 (2)
O1W—Gd1—O777.79 (6)C16—C15—H15B109.3
O2—Gd1—O776.98 (7)C9—C15—H15B109.3
O5—Gd1—O7140.79 (6)C16—C15—H15C109.3
O10—Gd1—O490.62 (6)C9—C15—H15C109.3
O1—Gd1—O475.77 (6)H15B—C15—H15C108.0
O1W—Gd1—O4126.62 (6)O5—C16—O4119.6 (2)
O2—Gd1—O472.53 (6)O5—C16—C15119.5 (2)
O5—Gd1—O451.99 (6)O4—C16—C15120.9 (2)
O7—Gd1—O4147.45 (6)O5—C16—Gd158.02 (13)
O10—Gd1—O866.00 (5)O4—C16—Gd162.29 (13)
O1—Gd1—O875.82 (5)C15—C16—Gd1169.50 (17)
O1W—Gd1—O873.47 (5)C18—C17—C22117.8 (3)
O2—Gd1—O8102.56 (6)C18—C17—C23120.9 (3)
O5—Gd1—O8139.94 (5)C22—C17—C23121.3 (3)
O7—Gd1—O851.47 (5)C17—C18—C19121.4 (3)
O4—Gd1—O8147.34 (5)C17—C18—H18B119.3
O10—Gd1—N1154.44 (6)C19—C18—H18B119.3
O1—Gd1—N1130.04 (6)C20—C19—C18119.8 (3)
O1W—Gd1—N181.33 (6)C20—C19—H19A120.1
O2—Gd1—N176.56 (6)C18—C19—H19A120.1
O5—Gd1—N173.68 (6)O9—C20—C19122.6 (3)
O7—Gd1—N174.93 (6)O9—C20—C21118.0 (2)
O4—Gd1—N187.01 (6)C19—C20—C21119.4 (3)
O8—Gd1—N1123.99 (6)C22—C21—C20120.2 (3)
O10—Gd1—C8100.05 (7)C22—C21—H21A119.9
O1—Gd1—C827.11 (6)C20—C21—H21A119.9
O1W—Gd1—C8163.63 (7)C21—C22—C17121.4 (3)
O2—Gd1—C826.73 (6)C21—C22—H22A119.3
O5—Gd1—C8121.57 (7)C17—C22—H22A119.3
O7—Gd1—C887.98 (7)C17—C23—C24111.9 (2)
O4—Gd1—C869.67 (7)C17—C23—H23A109.2
O8—Gd1—C891.37 (6)C24—C23—H23A109.2
N1—Gd1—C8102.93 (7)C17—C23—H23B109.2
O10—Gd1—C1689.89 (6)C24—C23—H23B109.2
O1—Gd1—C16100.66 (7)H23A—C23—H23B107.9
O1W—Gd1—C16100.77 (7)O7—C24—O8120.4 (2)
O2—Gd1—C1693.83 (7)O7—C24—C23120.3 (2)
O5—Gd1—C1625.99 (6)O8—C24—C23119.3 (2)
O7—Gd1—C16151.73 (6)O7—C24—Gd157.67 (13)
O4—Gd1—C1626.22 (6)O8—C24—Gd163.23 (12)
O8—Gd1—C16155.75 (6)C23—C24—Gd1171.66 (19)
N1—Gd1—C1676.94 (7)C30—C25—C26117.9 (2)
C8—Gd1—C1695.60 (8)C30—C25—C31120.0 (3)
O10—Gd1—C2491.87 (6)C26—C25—C31122.1 (3)
O1—Gd1—C2487.13 (7)C27—C26—C25121.2 (3)
O1W—Gd1—C2472.09 (7)C27—C26—H26A119.4
O2—Gd1—C2491.21 (7)C25—C26—H26A119.4
O5—Gd1—C24146.77 (6)C28—C27—C26119.6 (3)
O7—Gd1—C2425.30 (6)C28—C27—H27A120.2
O4—Gd1—C24161.24 (6)C26—C27—H27A120.2
O8—Gd1—C2426.31 (6)C27—C28—O12122.0 (2)
N1—Gd1—C2498.49 (7)C27—C28—C29120.3 (2)
C8—Gd1—C2491.59 (7)O12—C28—C29117.7 (2)
C16—Gd1—C24172.19 (7)C30—C29—C28119.5 (3)
O8—Gd2—O14128.23 (5)C30—C29—H29A120.3
O8—Gd2—O2W78.66 (6)C28—C29—H29A120.3
O14—Gd2—O2W143.57 (6)C29—C30—C25121.4 (3)
O8—Gd2—O1375.12 (5)C29—C30—H30A119.3
O14—Gd2—O1353.70 (6)C25—C30—H30A119.3
O2W—Gd2—O13147.68 (6)C32—C31—C25115.0 (2)
O8—Gd2—O1681.01 (6)C32—C31—H31A108.5
O14—Gd2—O16126.83 (6)C25—C31—H31A108.5
O2W—Gd2—O1675.76 (6)C32—C31—H31B108.5
O13—Gd2—O16117.69 (6)C25—C31—H31B108.5
O8—Gd2—O1798.64 (6)H31A—C31—H31B107.5
O14—Gd2—O1777.82 (6)O11—C32—O10119.4 (2)
O2W—Gd2—O17127.09 (6)O11—C32—C31122.7 (2)
O13—Gd2—O1775.88 (6)O10—C32—C31117.9 (2)
O16—Gd2—O1752.01 (6)O11—C32—Gd260.97 (12)
O8—Gd2—O1067.13 (5)O10—C32—Gd259.64 (12)
O14—Gd2—O1090.95 (6)C31—C32—Gd2168.77 (18)
O2W—Gd2—O1076.95 (6)C34—C33—C38117.4 (2)
O13—Gd2—O1075.66 (6)C34—C33—C39121.4 (2)
O16—Gd2—O10141.35 (5)C38—C33—C39121.2 (2)
O17—Gd2—O10150.66 (5)C33—C34—C35121.2 (2)
O8—Gd2—O11115.28 (5)C33—C34—H34A119.4
O14—Gd2—O1173.16 (6)C35—C34—H34A119.4
O2W—Gd2—O1172.69 (6)C36—C35—C34120.0 (2)
O13—Gd2—O11101.96 (6)C36—C35—H35A120.0
O16—Gd2—O11140.12 (6)C34—C35—H35A120.0
O17—Gd2—O11144.49 (6)O15—C36—C35122.8 (2)
O10—Gd2—O1150.57 (5)O15—C36—C37117.8 (2)
O8—Gd2—N3154.59 (6)C35—C36—C37119.4 (2)
O14—Gd2—N375.97 (6)C38—C37—C36119.9 (2)
O2W—Gd2—N383.92 (6)C38—C37—H37A120.0
O13—Gd2—N3126.60 (6)C36—C37—H37A120.0
O16—Gd2—N376.84 (6)C37—C38—C33122.0 (2)
O17—Gd2—N377.34 (6)C37—C38—H38A119.0
O10—Gd2—N3126.51 (6)C33—C38—H38A119.0
O11—Gd2—N376.15 (6)C33—C39—C40115.8 (2)
O8—Gd2—C40101.90 (6)C33—C39—H39A108.3
O14—Gd2—C4026.70 (6)C40—C39—H39A108.3
O2W—Gd2—C40157.94 (7)C33—C39—H39B108.3
O13—Gd2—C4027.00 (6)C40—C39—H39B108.3
O16—Gd2—C40126.27 (7)H39A—C39—H39B107.4
O17—Gd2—C4074.87 (6)O14—C40—O13119.9 (2)
O10—Gd2—C4082.95 (6)O14—C40—C39118.8 (2)
O11—Gd2—C4087.57 (7)O13—C40—C39121.3 (2)
N3—Gd2—C40101.18 (7)O14—C40—Gd259.66 (12)
O8—Gd2—C4891.76 (6)O13—C40—Gd260.29 (12)
O14—Gd2—C48101.95 (7)C39—C40—Gd2177.10 (18)
O2W—Gd2—C48100.94 (7)C42—C41—C46117.2 (2)
O13—Gd2—C4898.45 (7)C42—C41—C47120.9 (3)
O16—Gd2—C4825.90 (7)C46—C41—C47121.8 (3)
O17—Gd2—C4826.27 (6)C41—C42—C43121.8 (3)
O10—Gd2—C48158.86 (6)C41—C42—H42A119.1
O11—Gd2—C48149.45 (6)C43—C42—H42A119.1
N3—Gd2—C4873.45 (7)C44—C43—C42119.9 (3)
C40—Gd2—C48101.09 (7)C44—C43—H43A120.1
O8—Gd2—C3290.56 (6)C42—C43—H43A120.1
O14—Gd2—C3283.98 (7)O18—C44—C45117.8 (3)
O2W—Gd2—C3270.21 (6)O18—C44—C43122.8 (3)
O13—Gd2—C3291.34 (6)C45—C44—C43119.4 (3)
O16—Gd2—C32145.93 (6)C46—C45—C44119.8 (3)
O17—Gd2—C32161.63 (6)C46—C45—H45A120.1
O10—Gd2—C3225.68 (6)C44—C45—H45A120.1
O11—Gd2—C3225.21 (6)C45—C46—C41121.8 (3)
N3—Gd2—C32100.84 (6)C45—C46—H46A119.1
C40—Gd2—C3287.73 (7)C41—C46—H46A119.1
C48—Gd2—C32170.20 (7)C48—C47—C41111.9 (2)
C8—O1—Gd192.24 (14)C48—C47—H47A109.2
Gd1—O1W—H1WA132.3C41—C47—H47A109.2
Gd1—O1W—H1WB119.3C48—C47—H47B109.2
H1WA—O1W—H1WB107.7C41—C47—H47B109.2
C8—O2—Gd192.46 (15)H47A—C47—H47B107.9
Gd2—O2W—H2WA130.6O16—C48—O17119.5 (2)
Gd2—O2W—H2WB124.4O16—C48—C47119.9 (2)
H2WA—O2W—H2WB104.7O17—C48—C47120.6 (2)
C4—O3—H3109.5O16—C48—Gd258.53 (13)
C16—O4—Gd191.49 (15)O17—C48—Gd261.53 (13)
C16—O5—Gd195.99 (15)C47—C48—Gd2171.38 (17)
C12—O6—H6109.5N1—C49—C50123.6 (2)
C24—O7—Gd197.02 (15)N1—C49—H49A118.2
C24—O8—Gd2153.55 (16)C50—C49—H49A118.2
C24—O8—Gd190.46 (14)C49—C50—C51119.4 (3)
Gd2—O8—Gd1113.76 (6)C49—C50—H50A120.3
C20—O9—H9109.5C51—C50—H50A120.3
C32—O10—Gd1142.46 (15)C50—C51—C52117.2 (2)
C32—O10—Gd294.68 (14)C50—C51—C56121.7 (3)
Gd1—O10—Gd2113.11 (6)C52—C51—C56121.1 (2)
C32—O11—Gd293.81 (14)C53—C52—C51119.8 (2)
C28—O12—H12109.5C53—C52—H52A120.1
C40—O13—Gd292.71 (13)C51—C52—H52A120.1
C40—O14—Gd293.64 (15)N1—C53—C52123.3 (3)
C36—O15—H15109.5N1—C53—H53A118.4
C48—O16—Gd295.57 (15)C52—C53—H53A118.4
C48—O17—Gd292.20 (15)N2—C54—C55123.9 (3)
C44—O18—H18109.5N2—C54—H54A118.1
C49—N1—C53116.6 (2)C55—C54—H54A118.1
C49—N1—Gd1118.59 (16)C56—C55—C54119.4 (3)
C53—N1—Gd1124.45 (17)C56—C55—H55A120.3
C58—N2—C54115.9 (3)C54—C55—H55A120.3
C63—N3—C59116.2 (2)C57—C56—C55116.9 (3)
C63—N3—Gd2121.96 (16)C57—C56—C51122.1 (3)
C59—N3—Gd2121.48 (17)C55—C56—C51121.0 (3)
C64—N4—C68116.5 (3)C56—C57—C58119.3 (3)
C6—C1—C2117.5 (2)C56—C57—H57A120.4
C6—C1—C7121.6 (3)C58—C57—H57A120.4
C2—C1—C7120.9 (3)N2—C58—C57124.6 (3)
C3—C2—C1121.5 (3)N2—C58—H58A117.7
C3—C2—H2A119.3C57—C58—H58A117.7
C1—C2—H2A119.3N3—C59—C60123.2 (3)
C4—C3—C2120.1 (3)N3—C59—H59A118.4
C4—C3—H3B119.9C60—C59—H59A118.4
C2—C3—H3B119.9C59—C60—C61120.5 (2)
C5—C4—C3119.7 (2)C59—C60—H60A119.7
C5—C4—O3122.8 (2)C61—C60—H60A119.7
C3—C4—O3117.5 (2)C60—C61—C62116.2 (2)
C4—C5—C6119.6 (3)C60—C61—C66121.2 (2)
C4—C5—H5A120.2C62—C61—C66122.5 (3)
C6—C5—H5A120.2C63—C62—C61119.9 (3)
C1—C6—C5121.5 (3)C63—C62—H62A120.1
C1—C6—H6B119.2C61—C62—H62A120.1
C5—C6—H6B119.2N3—C63—C62123.9 (2)
C1—C7—C8115.9 (2)N3—C63—H63A118.1
C1—C7—H7A108.3C62—C63—H63A118.1
C8—C7—H7A108.3N4—C64—C65123.6 (4)
C1—C7—H7B108.3N4—C64—H64A118.2
C8—C7—H7B108.3C65—C64—H64A118.2
H7A—C7—H7B107.4C64—C65—C66119.7 (3)
O2—C8—O1120.7 (2)C64—C65—H65A120.1
O2—C8—C7119.5 (2)C66—C65—H65A120.1
O1—C8—C7119.8 (2)C67—C66—C65116.7 (3)
O2—C8—Gd160.81 (13)C67—C66—C61121.3 (3)
O1—C8—Gd160.65 (12)C65—C66—C61122.0 (3)
C7—C8—Gd1169.9 (2)C66—C67—C68119.3 (3)
C14—C9—C10117.8 (2)C66—C67—H67A120.3
C14—C9—C15122.3 (2)C68—C67—H67A120.3
C10—C9—C15119.8 (2)N4—C68—C67124.1 (4)
C11—C10—C9121.0 (3)N4—C68—H68A117.9
C11—C10—H10A119.5C67—C68—H68A117.9
C9—C10—H10A119.5H3WA—O3W—H3WB104.8
C12—C11—C10120.3 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WB···O130.772.002.744 (2)161
O1W—H1WA···N4i0.782.022.784 (3)167
O2W—H2WB···O10.822.002.750 (2)151
O2W—H2WA···N2ii0.832.032.842 (3)167
O3—H3···O3W0.821.862.641 (3)160
O6—H6···O12i0.821.942.743 (3)168
O9—H9···O17iii0.821.872.675 (3)167
O12—H12···O11iv0.821.942.750 (3)167
O15—H15···O3v0.821.902.717 (3)174
O18—H18···O9ii0.821.972.767 (3)162
O3W—H3WA···O4vi0.811.962.773 (3)179
O3W—H3WB···O6ii0.831.992.808 (3)165
Symmetry codes: (i) x, y1, z; (ii) x, y+1, z; (iii) x+2, y, z+1; (iv) x+2, y+1, z; (v) x+1, y1, z; (vi) x+1, y+1, z.

Experimental details

Crystal data
Chemical formula[Gd2(C8H7O3)6(C10H8N2)2(H2O)2]·H2O
Mr1587.73
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)11.7436 (1), 16.2654 (2), 18.4311 (2)
α, β, γ (°)83.52 (1), 72.11 (1), 71.10 (1)
V3)3169.4 (3)
Z2
Radiation typeMo Kα
µ (mm1)2.16
Crystal size (mm)0.15 × 0.13 × 0.12
Data collection
DiffractometerBruker APEXII area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.731, 0.772
No. of measured, independent and
observed [I > 2σ(I)] reflections
41430, 11119, 9631
Rint0.026
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.020, 0.048, 1.05
No. of reflections11117
No. of parameters862
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.45, 0.43

Computer programs: APEX2 (Bruker, 2006), SAINT (Bruker, 2006), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WB···O130.772.002.744 (2)160.9
O1W—H1WA···N4i0.782.022.784 (3)167.1
O2W—H2WB···O10.822.002.750 (2)151.1
O2W—H2WA···N2ii0.832.032.842 (3)167.4
O3—H3···O3W0.821.862.641 (3)159.7
O6—H6···O12i0.821.942.743 (3)167.9
O9—H9···O17iii0.821.872.675 (3)167.3
O12—H12···O11iv0.821.942.750 (3)167.4
O15—H15···O3v0.821.902.717 (3)173.6
O18—H18···O9ii0.821.972.767 (3)162.4
O3W—H3WA···O4vi0.811.962.773 (3)179.3
O3W—H3WB···O6ii0.831.992.808 (3)165.0
Symmetry codes: (i) x, y1, z; (ii) x, y+1, z; (iii) x+2, y, z+1; (iv) x+2, y+1, z; (v) x+1, y1, z; (vi) x+1, y+1, z.
 

References

First citationBruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationBurnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.  Google Scholar
First citationFang, R.-Q. & Zhang, X.-M. (2006). Inorg. Chem. 45, 4801–4810.  Web of Science CSD CrossRef PubMed CAS Google Scholar
First citationFarrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  CrossRef IUCr Journals Google Scholar
First citationFavas, M. C., Kepert, D. L., Skelton, B. W. & White, A. H. (1980). J. Chem. Soc. Dalton Trans. pp. 454–458.  CSD CrossRef Web of Science Google Scholar
First citationHatscher, S. T. (2005). Private Communication.  Google Scholar
First citationJohn, D. & Urland, W. (2006). Private Communication.  Google Scholar
First citationLiu, J.-L., Li, H.-Q. & Zhao, G.-L. (2010). Acta Cryst. E66, m9.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWang, G.-H., Lei, Y.-Q. & Wang, N. (2010). Cryst. Growth Des. 10, 4060–4067.  Google Scholar
First citationWang, X.-X. & Sevov, S. (2008). Inorg. Chem. 47, 1037–1043.  Web of Science CSD CrossRef PubMed CAS Google Scholar

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