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ISSN: 2056-9890

Tetra­aqua­bis­­(2,6-dihy­dr­oxy­benzoato-κO1)(2,6-dihy­dr­oxy­benzoato-κ2O1,O1′)gadolinium(III) dihydrate

aCollege of Chemistry and Material Science, Huaibei Normal University, Xiangshan, Huaibei 235000, People's Republic of China
*Correspondence e-mail: 363019204@qq.com

(Received 30 March 2011; accepted 28 April 2011; online 7 May 2011)

In the title compound, [Gd(C7H5O4)3(H2O)4]·2H2O, the GdIII ion shows a distorted square anti­prismatic coordination formed by four aqua ligands and four O atoms from the three 2,6-dihy­droxy­benzoate (L) ligands. Two L ligands coordinate the GdIII ion in a monodentate mode, while the third coordinates it in a bidentate–chelating coordination mode. An extensive three-dimensional O—H⋯O hydrogen-bonding network consolidates the crystal packing.

Related literature

The crystal structures of related complexes with Ho and Tb were reported by Glowiak et al. (1999[Glowiak, T., Brzyska, W., Kula, A. & Rzaczynska, Z. (1999). J. Coord. Chem. 48, 477-486.]).

[Scheme 1]

Experimental

Crystal data
  • [Gd(C7H5O4)3(H2O)4]·2H2O

  • Mr = 724.68

  • Triclinic, [P \overline 1]

  • a = 10.7666 (4) Å

  • b = 11.3289 (4) Å

  • c = 12.4741 (4) Å

  • α = 82.270 (1)°

  • β = 73.066 (1)°

  • γ = 68.178 (1)°

  • V = 1350.65 (8) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 2.54 mm−1

  • T = 294 K

  • 0.24 × 0.20 × 0.18 mm

Data collection
  • Bruker APEXII area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2007[Bruker (2007). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.581, Tmax = 0.658

  • 6854 measured reflections

  • 4691 independent reflections

  • 4301 reflections with I > 2σ(I)

  • Rint = 0.014

Refinement
  • R[F2 > 2σ(F2)] = 0.022

  • wR(F2) = 0.052

  • S = 1.04

  • 4691 reflections

  • 415 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.48 e Å−3

  • Δρmin = −0.61 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O13—H13A⋯O17i 0.84 (5) 1.88 (5) 2.697 (5) 161 (4)
O14—H14A⋯O17i 0.77 (5) 1.99 (7) 2.766 (5) 172 (4)
O15—H15A⋯O4ii 0.83 (5) 1.90 (8) 2.739 (5) 176 (5)
O16—H16A⋯O11 0.72 (4) 2.09 (5) 2.735 (5) 151 (2)
O16—H16A⋯O12iii 0.72 (4) 2.50 (5) 2.865 (5) 113 (7)
O17—H17A⋯O18 0.86 (5) 1.81 (5) 2.668 (5) 175 (5)
O18—H18A⋯O5ii 0.91 (7) 1.88 (5) 2.752 (5) 161 (4)
O13—H13B⋯O1iv 0.88 (5) 1.94 (5) 2.808 (5) 172 (5)
O14—H14B⋯O9v 0.84 (5) 1.90 (5) 2.739 (5) 174 (5)
O15—H15B⋯O18 0.70 (4) 2.22 (5) 2.917 (5) 176 (6)
O16—H16B⋯O2 0.88 (6) 1.89 (5) 2.672 (5) 147 (5)
O17—H17B⋯O8vi 0.82 (5) 2.03 (5) 2.713 (5) 140 (5)
O18—H18B⋯O12iii 0.83 (5) 2.08 (5) 2.898 (5) 172 (3)
O1—H1⋯O2 0.82 1.78 2.515 (5) 148
O4—H4⋯O3 0.82 1.82 2.549 (5) 147
O5—H5⋯O6 0.82 1.83 2.566 (5) 148
O8—H8⋯O7 0.82 1.83 2.546 (5) 145
O9—H9⋯O10 0.82 1.82 2.551 (5) 147
O12—H12⋯O11 0.82 1.78 2.512 (5) 148
Symmetry codes: (i) x+1, y, z; (ii) -x+1, -y+2, -z+1; (iii) -x+1, -y+1, -z+2; (iv) -x+1, -y+2, -z+2; (v) -x+2, -y+1, -z+1; (vi) -x+1, -y+1, -z+1.

Data collection: SMART (Bruker, 2007[Bruker (2007). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2007[Bruker (2007). SMART, SAINT and SADABS. 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL and publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information


Comment top

The title compound is isomorphous with the related Ho and Tb complexes (Glowiak et al., 1999). The coordinating Gd—O bond lengths are in the range 2.344 (2)–2.512 (2) Å. Intermolecular O—H···O hydrogen bonds (Table 1) form an extensive three-dimensional hydrogen-bonding network, which consolidate the crystal packing.

Related literature top

he crystal structures of related complexes with Ho and Tb were reported by Glowiak et al. (1999).

Experimental top

The title complex was synthesized by dissolving 2,6-dihydroxybenzoic acid (10 mmol, 1.54 g) in 25 ml of ethanol. This was followed by the addition of Gadolinium nitrate (3 mmol,1.35 g), dissolved in 20 ml of distilled water. The mixture was stirred at room temperature for 5 h and the resulting white precipitate was filtered, dried and recrystallized from water.

Refinement top

C-bound H atoms were geometrically positioned and refined as riding, with C—H = 0.93 Å and Uiso(H) = 1.2 Ueq(C). H atoms attached to O atoms were found in a difference Fourier map and isotropically refined.

Computing details top

Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound, drawn with 50% probability displacement ellipsoids. H atoms omitted for clarity.
Tetraaquabis(2,6-dihydroxybenzoato-κO1)(2,6-dihydroxybenzoato- κ2O1,O1')gadolinium(III) dihydrate top
Crystal data top
[Gd(C7H5O4)3(H2O)4]·2H2OV = 1350.65 (8) Å3
Mr = 724.68Z = 2
Triclinic, P1F(000) = 722
Hall symbol: -P 1Dx = 1.782 Mg m3
a = 10.7666 (4) ÅMelting point: 476 K
b = 11.3289 (4) ÅMo Kα radiation, λ = 0.71073 Å
c = 12.4741 (4) ŵ = 2.54 mm1
α = 82.270 (1)°T = 294 K
β = 73.066 (1)°Block, white
γ = 68.178 (1)°0.24 × 0.20 × 0.18 mm
Data collection top
Bruker APEXII area-detector
diffractometer
4691 independent reflections
Radiation source: fine-focus sealed tube4301 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.014
ω scansθmax = 25.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2007)
h = 1212
Tmin = 0.581, Tmax = 0.658k = 1013
6854 measured reflectionsl = 1414
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)] = 0.022Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.052H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.0247P)2 + 0.6501P]
where P = (Fo2 + 2Fc2)/3
4691 reflections(Δ/σ)max = 0.002
415 parametersΔρmax = 0.48 e Å3
0 restraintsΔρmin = 0.61 e Å3
Crystal data top
[Gd(C7H5O4)3(H2O)4]·2H2Oγ = 68.178 (1)°
Mr = 724.68V = 1350.65 (8) Å3
Triclinic, P1Z = 2
a = 10.7666 (4) ÅMo Kα radiation
b = 11.3289 (4) ŵ = 2.54 mm1
c = 12.4741 (4) ÅT = 294 K
α = 82.270 (1)°0.24 × 0.20 × 0.18 mm
β = 73.066 (1)°
Data collection top
Bruker APEXII area-detector
diffractometer
4691 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2007)
4301 reflections with I > 2σ(I)
Tmin = 0.581, Tmax = 0.658Rint = 0.014
6854 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0220 restraints
wR(F2) = 0.052H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 0.48 e Å3
4691 reflectionsΔρmin = 0.61 e Å3
415 parameters
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*/Ueq
C10.5308 (3)1.0415 (3)0.7814 (2)0.0340 (7)
C20.4935 (3)1.1804 (3)0.7630 (2)0.0332 (7)
C30.5284 (3)1.2357 (3)0.6563 (3)0.0377 (8)
C40.4932 (4)1.3661 (3)0.6407 (3)0.0508 (9)
H4A0.51641.40180.56950.061*
C50.4231 (4)1.4428 (3)0.7326 (3)0.0542 (10)
H5A0.40051.53040.72250.065*
C60.3861 (4)1.3924 (3)0.8387 (3)0.0477 (9)
H60.33841.44540.89950.057*
C70.4203 (3)1.2626 (3)0.8539 (3)0.0365 (7)
C80.7815 (4)0.7434 (3)0.4254 (2)0.0365 (7)
C90.8391 (3)0.7349 (3)0.3029 (3)0.0370 (7)
C100.9056 (4)0.6168 (3)0.2523 (3)0.0452 (9)
C110.9649 (4)0.6091 (4)0.1376 (3)0.0570 (10)
H111.00970.53040.10420.068*
C120.9566 (5)0.7183 (5)0.0745 (3)0.0635 (12)
H12A0.99730.71250.00220.076*
C130.8907 (4)0.8359 (4)0.1199 (3)0.0597 (11)
H130.88560.90890.07460.072*
C140.8314 (4)0.8445 (3)0.2349 (3)0.0455 (9)
C150.7184 (3)0.4653 (3)0.7986 (2)0.0350 (7)
C160.7694 (3)0.3260 (3)0.7872 (3)0.0332 (7)
C170.8403 (4)0.2674 (3)0.6841 (3)0.0403 (8)
C180.8838 (4)0.1373 (3)0.6746 (3)0.0540 (10)
H180.93100.09980.60550.065*
C190.8556 (4)0.0642 (4)0.7698 (4)0.0604 (11)
H190.88380.02340.76400.072*
C200.7869 (4)0.1174 (4)0.8733 (4)0.0564 (10)
H200.76910.06610.93640.068*
C210.7448 (4)0.2473 (3)0.8828 (3)0.0404 (8)
Gd10.702869 (16)0.750791 (13)0.665777 (11)0.02894 (6)
H13A0.877 (5)0.730 (4)0.821 (4)0.069 (15)*
H14A0.971 (5)0.755 (5)0.642 (4)0.079 (18)*
H15A0.467 (4)0.786 (4)0.568 (4)0.062 (13)*
H16A0.535 (4)0.704 (4)0.867 (3)0.046 (14)*
H17A0.122 (5)0.744 (4)0.776 (4)0.085 (17)*
H18A0.228 (7)0.883 (7)0.793 (6)0.15 (3)*
H13B0.745 (5)0.750 (4)0.894 (4)0.087 (16)*
H14B0.991 (5)0.729 (4)0.543 (4)0.087 (17)*
H15B0.437 (5)0.772 (4)0.668 (4)0.059 (16)*
H16B0.494 (6)0.831 (5)0.872 (5)0.11 (2)*
H17B0.108 (5)0.637 (5)0.750 (4)0.081 (17)*
H18B0.265 (5)0.779 (4)0.868 (4)0.081 (17)*
O10.3847 (3)1.2146 (2)0.95957 (18)0.0484 (6)
H10.41281.13670.95840.073*
O20.4931 (3)0.9972 (2)0.87718 (18)0.0518 (7)
O30.6016 (2)0.96988 (19)0.69634 (16)0.0388 (5)
O40.5976 (3)1.1625 (2)0.56387 (17)0.0483 (6)
H40.61861.08710.58330.072*
O50.7661 (3)0.9615 (2)0.2789 (2)0.0672 (8)
H50.73390.95460.34660.101*
O60.7188 (3)0.8501 (2)0.47171 (18)0.0468 (6)
O70.7986 (3)0.6422 (2)0.48681 (17)0.0439 (6)
O80.9160 (3)0.5071 (2)0.3133 (2)0.0652 (8)
H80.87060.52330.37830.098*
O90.8689 (3)0.3387 (2)0.58862 (18)0.0538 (7)
H90.83250.41440.60290.081*
O100.7447 (2)0.53404 (19)0.71024 (16)0.0380 (5)
O110.6501 (3)0.5131 (2)0.89201 (18)0.0520 (7)
O120.6791 (3)0.2971 (2)0.98503 (19)0.0577 (7)
H120.65920.37460.97990.087*
O130.7942 (3)0.7430 (2)0.8236 (2)0.0445 (6)
O140.9283 (3)0.7671 (3)0.5988 (2)0.0478 (6)
O150.4977 (3)0.7588 (3)0.6240 (3)0.0486 (7)
O160.5253 (3)0.7617 (3)0.8331 (2)0.0411 (6)
O170.0657 (3)0.7124 (3)0.7653 (2)0.0562 (7)
O180.2460 (3)0.7987 (3)0.8066 (3)0.0568 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0415 (19)0.0323 (17)0.0258 (16)0.0083 (14)0.0103 (14)0.0029 (13)
C20.0367 (18)0.0332 (17)0.0284 (16)0.0069 (14)0.0130 (13)0.0023 (13)
C30.042 (2)0.0387 (18)0.0308 (17)0.0090 (15)0.0138 (14)0.0003 (14)
C40.067 (3)0.041 (2)0.042 (2)0.0171 (19)0.0187 (18)0.0097 (16)
C50.064 (3)0.0315 (19)0.063 (3)0.0087 (18)0.022 (2)0.0003 (17)
C60.052 (2)0.038 (2)0.049 (2)0.0056 (17)0.0154 (18)0.0134 (16)
C70.042 (2)0.0345 (18)0.0318 (17)0.0081 (15)0.0135 (14)0.0057 (13)
C80.045 (2)0.0417 (19)0.0239 (15)0.0192 (16)0.0054 (14)0.0017 (14)
C90.0374 (19)0.050 (2)0.0244 (15)0.0190 (16)0.0058 (13)0.0009 (14)
C100.054 (2)0.056 (2)0.0294 (17)0.0244 (19)0.0073 (16)0.0090 (16)
C110.068 (3)0.070 (3)0.0319 (19)0.027 (2)0.0029 (18)0.0148 (19)
C120.065 (3)0.105 (4)0.0235 (18)0.037 (3)0.0052 (18)0.005 (2)
C130.063 (3)0.081 (3)0.0317 (19)0.030 (2)0.0108 (18)0.020 (2)
C140.052 (2)0.050 (2)0.0336 (18)0.0190 (18)0.0118 (16)0.0075 (16)
C150.0389 (19)0.0349 (17)0.0276 (16)0.0133 (14)0.0046 (14)0.0025 (13)
C160.0327 (18)0.0315 (17)0.0342 (17)0.0127 (14)0.0059 (14)0.0010 (13)
C170.0373 (19)0.0349 (18)0.0434 (19)0.0106 (15)0.0044 (15)0.0038 (15)
C180.052 (2)0.041 (2)0.059 (2)0.0087 (18)0.0056 (19)0.0128 (18)
C190.063 (3)0.0304 (19)0.088 (3)0.0133 (19)0.024 (2)0.002 (2)
C200.062 (3)0.042 (2)0.069 (3)0.0244 (19)0.026 (2)0.023 (2)
C210.046 (2)0.042 (2)0.0365 (18)0.0207 (16)0.0128 (16)0.0112 (15)
Gd10.03710 (10)0.02723 (9)0.01941 (8)0.01211 (7)0.00154 (6)0.00127 (6)
O10.0634 (17)0.0415 (14)0.0304 (12)0.0094 (13)0.0058 (11)0.0097 (10)
O20.083 (2)0.0354 (13)0.0248 (12)0.0148 (13)0.0049 (12)0.0002 (10)
O30.0524 (15)0.0315 (12)0.0253 (11)0.0092 (10)0.0056 (10)0.0034 (9)
O40.0705 (18)0.0412 (14)0.0250 (11)0.0128 (13)0.0109 (11)0.0023 (10)
O50.089 (2)0.0483 (16)0.0426 (15)0.0147 (15)0.0049 (15)0.0146 (12)
O60.0646 (17)0.0373 (13)0.0286 (12)0.0137 (12)0.0031 (11)0.0006 (10)
O70.0685 (17)0.0356 (13)0.0244 (11)0.0211 (12)0.0041 (11)0.0006 (10)
O80.104 (3)0.0460 (16)0.0382 (14)0.0290 (16)0.0009 (15)0.0107 (12)
O90.0708 (19)0.0442 (14)0.0305 (12)0.0174 (14)0.0089 (12)0.0068 (11)
O100.0517 (14)0.0314 (12)0.0242 (11)0.0150 (10)0.0007 (10)0.0020 (9)
O110.0757 (19)0.0404 (14)0.0274 (12)0.0186 (13)0.0032 (12)0.0027 (10)
O120.078 (2)0.0539 (16)0.0328 (13)0.0260 (15)0.0044 (13)0.0136 (11)
O130.0400 (15)0.0621 (17)0.0298 (13)0.0185 (13)0.0047 (11)0.0047 (11)
O140.0431 (16)0.0630 (18)0.0321 (14)0.0193 (13)0.0007 (13)0.0057 (13)
O150.0488 (18)0.0697 (19)0.0293 (14)0.0218 (14)0.0128 (14)0.0000 (13)
O160.0433 (15)0.0522 (17)0.0260 (12)0.0206 (13)0.0019 (10)0.0002 (13)
O170.0467 (17)0.0580 (19)0.0679 (19)0.0180 (15)0.0125 (14)0.0215 (15)
O180.0658 (19)0.0581 (19)0.0603 (19)0.0311 (15)0.0308 (15)0.0126 (15)
Geometric parameters (Å, º) top
C1—O21.245 (4)C17—C181.381 (5)
C1—O31.290 (3)C18—C191.378 (5)
C1—C21.475 (4)C18—H180.9300
C2—C31.402 (4)C19—C201.378 (6)
C2—C71.412 (4)C19—H190.9300
C3—O41.367 (4)C20—C211.380 (5)
C3—C41.383 (4)C20—H200.9300
C4—C51.384 (5)C21—O121.348 (4)
C4—H4A0.9300Gd1—O32.344 (2)
C5—C61.377 (5)Gd1—O102.345 (2)
C5—H5A0.9300Gd1—O162.366 (2)
C6—C71.377 (4)Gd1—O152.380 (3)
C6—H60.9300Gd1—O142.394 (3)
C7—O11.360 (4)Gd1—O132.422 (2)
C8—O61.267 (4)Gd1—O72.453 (2)
C8—O71.275 (4)Gd1—O62.515 (2)
C8—C91.474 (4)O1—H10.8200
C9—C141.396 (5)O4—H40.8200
C9—C101.398 (5)O5—H50.8200
C10—O81.351 (4)O8—H80.8200
C10—C111.386 (5)O9—H90.8200
C11—C121.362 (6)O12—H120.8200
C11—H110.9300O13—H13A0.84 (5)
C12—C131.365 (6)O13—H13B0.88 (5)
C12—H12A0.9300O14—H14A0.77 (5)
C13—C141.390 (5)O14—H14B0.84 (5)
C13—H130.9300O15—H15A0.83 (5)
C14—O51.353 (4)O15—H15B0.70 (4)
C15—O111.251 (4)O16—H16A0.72 (4)
C15—O101.286 (3)O16—H16B0.88 (6)
C15—C161.478 (4)O17—H17A0.86 (5)
C16—C171.399 (4)O17—H17B0.82 (5)
C16—C211.411 (4)O18—H18A0.91 (7)
C17—O91.370 (4)O18—H18B0.83 (5)
O2—C1—O3122.3 (3)C19—C20—H20120.2
O2—C1—C2119.6 (3)C21—C20—H20120.2
O3—C1—C2118.1 (3)O12—C21—C20118.5 (3)
C3—C2—C7117.6 (3)O12—C21—C16120.9 (3)
C3—C2—C1122.1 (3)C20—C21—C16120.6 (3)
C7—C2—C1120.4 (3)O3—Gd1—O10156.25 (7)
O4—C3—C4117.8 (3)O3—Gd1—O1677.50 (10)
O4—C3—C2121.0 (3)O10—Gd1—O1679.15 (10)
C4—C3—C2121.2 (3)O3—Gd1—O1588.85 (9)
C3—C4—C5119.1 (3)O10—Gd1—O1587.16 (9)
C3—C4—H4A120.4O16—Gd1—O1569.80 (10)
C5—C4—H4A120.4O3—Gd1—O1490.77 (9)
C6—C5—C4121.5 (3)O10—Gd1—O14104.82 (9)
C6—C5—H5A119.2O16—Gd1—O14141.00 (10)
C4—C5—H5A119.2O15—Gd1—O14147.97 (11)
C5—C6—C7119.3 (3)O3—Gd1—O1384.56 (8)
C5—C6—H6120.4O10—Gd1—O1383.92 (8)
C7—C6—H6120.4O16—Gd1—O1371.30 (9)
O1—C7—C6118.4 (3)O15—Gd1—O13141.05 (10)
O1—C7—C2120.3 (3)O14—Gd1—O1370.64 (10)
C6—C7—C2121.3 (3)O3—Gd1—O7128.31 (7)
O6—C8—O7118.9 (3)O10—Gd1—O773.64 (7)
O6—C8—C9121.2 (3)O16—Gd1—O7138.91 (9)
O7—C8—C9119.8 (3)O15—Gd1—O778.57 (10)
C14—C9—C10118.4 (3)O14—Gd1—O776.67 (9)
C14—C9—C8120.8 (3)O13—Gd1—O7133.70 (9)
C10—C9—C8120.8 (3)O3—Gd1—O676.04 (7)
O8—C10—C11118.1 (3)O10—Gd1—O6125.25 (7)
O8—C10—C9121.4 (3)O16—Gd1—O6136.37 (9)
C11—C10—C9120.5 (3)O15—Gd1—O675.59 (10)
C12—C11—C10119.2 (4)O14—Gd1—O673.26 (9)
C12—C11—H11120.4O13—Gd1—O6138.47 (9)
C10—C11—H11120.4O7—Gd1—O652.28 (7)
C11—C12—C13122.4 (3)C7—O1—H1109.5
C11—C12—H12A118.8C1—O3—Gd1136.40 (19)
C13—C12—H12A118.8C3—O4—H4109.5
C12—C13—C14118.8 (4)C14—O5—H5109.5
C12—C13—H13120.6C8—O6—Gd192.90 (18)
C14—C13—H13120.6C8—O7—Gd195.61 (18)
O5—C14—C13118.3 (3)C10—O8—H8109.5
O5—C14—C9121.0 (3)C17—O9—H9109.5
C13—C14—C9120.6 (4)C15—O10—Gd1136.89 (19)
O11—C15—O10122.0 (3)C21—O12—H12109.5
O11—C15—C16120.0 (3)Gd1—O13—H13A126 (3)
O10—C15—C16118.0 (3)Gd1—O13—H13B124 (3)
C17—C16—C21117.8 (3)H13A—O13—H13B110 (4)
C17—C16—C15122.6 (3)Gd1—O14—H14A118 (4)
C21—C16—C15119.6 (3)Gd1—O14—H14B126 (3)
O9—C17—C18117.8 (3)H14A—O14—H14B100 (5)
O9—C17—C16120.4 (3)Gd1—O15—H15A132 (3)
C18—C17—C16121.8 (3)Gd1—O15—H15B118 (4)
C19—C18—C17118.6 (4)H15A—O15—H15B102 (5)
C19—C18—H18120.7Gd1—O16—H16A115 (3)
C17—C18—H18120.7Gd1—O16—H16B117 (4)
C18—C19—C20121.8 (3)H16A—O16—H16B114 (5)
C18—C19—H19119.1H17A—O17—H17B109 (5)
C20—C19—H19119.1H18A—O18—H18B109 (5)
C19—C20—C21119.5 (3)
O2—C1—C2—C3177.4 (3)C16—C17—C18—C190.1 (6)
O3—C1—C2—C32.3 (5)C17—C18—C19—C200.6 (6)
O2—C1—C2—C72.5 (5)C18—C19—C20—C210.0 (6)
O3—C1—C2—C7177.8 (3)C19—C20—C21—O12179.3 (4)
C7—C2—C3—O4179.1 (3)C19—C20—C21—C161.1 (6)
C1—C2—C3—O40.8 (5)C17—C16—C21—O12178.9 (3)
C7—C2—C3—C40.5 (5)C15—C16—C21—O122.1 (5)
C1—C2—C3—C4179.6 (3)C17—C16—C21—C201.5 (5)
O4—C3—C4—C5180.0 (3)C15—C16—C21—C20177.6 (3)
C2—C3—C4—C50.4 (5)O2—C1—O3—Gd14.0 (5)
C3—C4—C5—C60.9 (6)C2—C1—O3—Gd1176.3 (2)
C4—C5—C6—C70.4 (6)O10—Gd1—O3—C113.5 (4)
C5—C6—C7—O1179.0 (3)O16—Gd1—O3—C124.3 (3)
C5—C6—C7—C20.5 (5)O15—Gd1—O3—C193.8 (3)
C3—C2—C7—O1179.4 (3)O14—Gd1—O3—C1118.2 (3)
C1—C2—C7—O10.7 (5)O13—Gd1—O3—C147.8 (3)
C3—C2—C7—C60.9 (5)O7—Gd1—O3—C1168.2 (3)
C1—C2—C7—C6179.2 (3)O6—Gd1—O3—C1169.2 (3)
O6—C8—C9—C142.9 (5)O7—C8—O6—Gd15.2 (3)
O7—C8—C9—C14174.8 (3)C9—C8—O6—Gd1172.5 (3)
O6—C8—C9—C10178.7 (3)O3—Gd1—O6—C8178.0 (2)
O7—C8—C9—C103.7 (5)O10—Gd1—O6—C813.7 (2)
C14—C9—C10—O8179.8 (3)O16—Gd1—O6—C8127.7 (2)
C8—C9—C10—O81.8 (5)O15—Gd1—O6—C889.5 (2)
C14—C9—C10—C111.3 (5)O14—Gd1—O6—C882.9 (2)
C8—C9—C10—C11177.1 (3)O13—Gd1—O6—C8113.4 (2)
O8—C10—C11—C12179.5 (4)O7—Gd1—O6—C82.98 (18)
C9—C10—C11—C120.5 (6)O6—C8—O7—Gd15.3 (3)
C10—C11—C12—C130.6 (6)C9—C8—O7—Gd1172.4 (3)
C11—C12—C13—C140.9 (7)O3—Gd1—O7—C84.2 (2)
C12—C13—C14—O5179.9 (4)O10—Gd1—O7—C8173.9 (2)
C12—C13—C14—C90.0 (6)O16—Gd1—O7—C8123.3 (2)
C10—C9—C14—O5178.8 (3)O15—Gd1—O7—C883.5 (2)
C8—C9—C14—O52.8 (5)O14—Gd1—O7—C876.0 (2)
C10—C9—C14—C131.1 (5)O13—Gd1—O7—C8121.8 (2)
C8—C9—C14—C13177.4 (3)O6—Gd1—O7—C82.98 (19)
O11—C15—C16—C17176.8 (3)O11—C15—O10—Gd12.3 (5)
O10—C15—C16—C172.2 (5)C16—C15—O10—Gd1178.7 (2)
O11—C15—C16—C212.3 (5)O3—Gd1—O10—C1512.1 (4)
O10—C15—C16—C21178.8 (3)O16—Gd1—O10—C1522.7 (3)
C21—C16—C17—O9179.1 (3)O15—Gd1—O10—C1592.7 (3)
C15—C16—C17—O91.8 (5)O14—Gd1—O10—C15117.4 (3)
C21—C16—C17—C180.9 (5)O13—Gd1—O10—C1549.3 (3)
C15—C16—C17—C18178.2 (3)O7—Gd1—O10—C15171.6 (3)
O9—C17—C18—C19179.9 (4)O6—Gd1—O10—C15162.8 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O13—H13A···O17i0.84 (5)1.88 (5)2.697 (5)161 (4)
O14—H14A···O17i0.77 (5)1.99 (7)2.766 (5)172 (4)
O15—H15A···O4ii0.83 (5)1.90 (8)2.739 (5)176 (5)
O16—H16A···O110.72 (4)2.09 (5)2.735 (5)151 (2)
O16—H16A···O12iii0.72 (4)2.50 (5)2.865 (5)113 (7)
O17—H17A···O180.86 (5)1.81 (5)2.668 (5)175 (5)
O18—H18A···O5ii0.91 (7)1.88 (5)2.752 (5)161 (4)
O13—H13B···O1iv0.88 (5)1.94 (5)2.808 (5)172 (5)
O14—H14B···O9v0.84 (5)1.90 (5)2.739 (5)174 (5)
O15—H15B···O180.70 (4)2.22 (5)2.917 (5)176 (6)
O16—H16B···O20.88 (6)1.89 (5)2.672 (5)147 (5)
O17—H17B···O8vi0.82 (5)2.03 (5)2.713 (5)140 (5)
O18—H18B···O12iii0.83 (5)2.08 (5)2.898 (5)172 (3)
O1—H1···O20.821.782.515 (5)148
O4—H4···O30.821.822.549 (5)147
O5—H5···O60.821.832.566 (5)148
O8—H8···O70.821.832.546 (5)145
O9—H9···O100.821.822.551 (5)147
O12—H12···O110.821.782.512 (5)148
Symmetry codes: (i) x+1, y, z; (ii) x+1, y+2, z+1; (iii) x+1, y+1, z+2; (iv) x+1, y+2, z+2; (v) x+2, y+1, z+1; (vi) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formula[Gd(C7H5O4)3(H2O)4]·2H2O
Mr724.68
Crystal system, space groupTriclinic, P1
Temperature (K)294
a, b, c (Å)10.7666 (4), 11.3289 (4), 12.4741 (4)
α, β, γ (°)82.270 (1), 73.066 (1), 68.178 (1)
V3)1350.65 (8)
Z2
Radiation typeMo Kα
µ (mm1)2.54
Crystal size (mm)0.24 × 0.20 × 0.18
Data collection
DiffractometerBruker APEXII area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2007)
Tmin, Tmax0.581, 0.658
No. of measured, independent and
observed [I > 2σ(I)] reflections
6854, 4691, 4301
Rint0.014
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.022, 0.052, 1.04
No. of reflections4691
No. of parameters415
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.48, 0.61

Computer programs: SMART (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O13—H13A···O17i0.84 (5)1.88 (5)2.697 (5)161 (4)
O14—H14A···O17i0.77 (5)1.99 (7)2.766 (5)172 (4)
O15—H15A···O4ii0.83 (5)1.90 (8)2.739 (5)176 (5)
O16—H16A···O110.72 (4)2.09 (5)2.735 (5)151 (2)
O16—H16A···O12iii0.72 (4)2.50 (5)2.865 (5)113 (7)
O17—H17A···O180.86 (5)1.81 (5)2.668 (5)175 (5)
O18—H18A···O5ii0.91 (7)1.88 (5)2.752 (5)161 (4)
O13—H13B···O1iv0.88 (5)1.94 (5)2.808 (5)172 (5)
O14—H14B···O9v0.84 (5)1.90 (5)2.739 (5)174 (5)
O15—H15B···O180.70 (4)2.22 (5)2.917 (5)176 (6)
O16—H16B···O20.88 (6)1.89 (5)2.672 (5)147 (5)
O17—H17B···O8vi0.82 (5)2.03 (5)2.713 (5)140 (5)
O18—H18B···O12iii0.83 (5)2.08 (5)2.898 (5)172 (3)
O1—H1···O20.821.782.515 (5)148
O4—H4···O30.821.822.549 (5)147
O5—H5···O60.821.832.566 (5)148
O8—H8···O70.821.832.546 (5)145
O9—H9···O100.821.822.551 (5)147
O12—H12···O110.821.782.512 (5)148
Symmetry codes: (i) x+1, y, z; (ii) x+1, y+2, z+1; (iii) x+1, y+1, z+2; (iv) x+1, y+2, z+2; (v) x+2, y+1, z+1; (vi) x+1, y+1, z+1.
 

Acknowledgements

Financial support from Huaibei Normal University is gratefully acknowledged

References

First citationBruker (2007). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationGlowiak, T., Brzyska, W., Kula, A. & Rzaczynska, Z. (1999). J. Coord. Chem. 48, 477–486.  CrossRef CAS Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWestrip, S. P. (2010). J. Appl. Cryst. 43, 920–925.  Web of Science CrossRef CAS IUCr Journals Google Scholar

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