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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 7| July 2010| Pages m740-m741

(4-Amino­benzene­sulfonato)­hepta­aqua­gadolinium(III) 4-amino­benzene­sulfonate nitrate 4,4′-bi­pyridyl tetra­solvate dihydrate

aShandong Provincial Key Laboratory of Microbial Engineering, Shandong Institute of Light Industry, Jinan 250353, People's Republic of China
*Correspondence e-mail: lujianghao001@yahoo.com.cn

(Received 17 May 2010; accepted 30 May 2010; online 5 June 2010)

In the title compound, [Gd(C6H6O3S)(H2O)7](C6H6O3S)(NO3)·4C10H8N2·2H2O, the GdIII ion is octa­coordinated by seven water mol­ecules and one O-bonded 4-amino­benzene­sulfonate anion in a square-anti­prismatic arrangement. In the crystal, the components are linked by N—H⋯O, O—H⋯N and O—H⋯O hydrogen bonds.

Related literature

For background to lanthanide coordination networks, see: Karthikeyan et al. (1989[Karthikeyan, S., Ryan, R. R. & Paine, R. T. (1989). Inorg. Chem. 28, 2783-2789.]).

[Scheme 1]

Experimental

Crystal data
  • [Gd(C6H6O3S)(H2O)7](C6H6O3S)(NO3)·4C10H8N2·2H2O

  • Mr = 1350.50

  • Orthorhombic, A b a 2

  • a = 33.529 (2) Å

  • b = 23.3375 (10) Å

  • c = 15.2046 (10) Å

  • V = 11897.3 (12) Å3

  • Z = 8

  • Mo Kα radiation

  • μ = 1.26 mm−1

  • T = 296 K

  • 0.12 × 0.10 × 0.08 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.863, Tmax = 0.906

  • 41191 measured reflections

  • 10477 independent reflections

  • 8881 reflections with I > 2σ(I)

  • Rint = 0.045

Refinement
  • R[F2 > 2σ(F2)] = 0.036

  • wR(F2) = 0.088

  • S = 1.00

  • 10477 reflections

  • 811 parameters

  • 27 restraints

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

  • Δρmax = 0.35 e Å−3

  • Δρmin = −0.53 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 5009 Friedel pairs

  • Flack parameter: 0.002 (1)

Table 1
Selected bond lengths (Å)

Gd1—O6W 2.375 (4)
Gd1—O2W 2.373 (4)
Gd1—O1W 2.389 (4)
Gd1—O3W 2.392 (4)
Gd1—O7W 2.391 (4)
Gd1—O5W 2.401 (4)
Gd1—O1 2.434 (4)
Gd1—O4W 2.440 (4)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O1W—H1W⋯N6 0.82 (2) 2.12 (2) 2.770 (7) 136 (3)
O1W—H2W⋯O5 0.82 (2) 2.13 (1) 2.759 (6) 134 (3)
O2W—H3W⋯O8W 0.82 (2) 1.93 (1) 2.657 (7) 147 (2)
O3W—H6W⋯N8 0.82 (2) 1.99 (1) 2.728 (7) 149 (2)
O4W—H8W⋯N9i 0.82 (2) 2.19 (2) 2.807 (7) 133 (1)
O5W—H9W⋯N4ii 0.82 (1) 1.86 (1) 2.647 (7) 159 (2)
O5W—H10W⋯O3 0.82 (2) 2.51 (2) 3.236 (6) 148 (4)
O5W—H10W⋯O1 0.82 (2) 2.50 (3) 2.931 (5) 114 (2)
O6W—H11W⋯O3iii 0.82 (3) 1.95 (3) 2.765 (6) 175 (5)
O6W—H12W⋯N3 0.82 (1) 1.90 (1) 2.719 (7) 178 (8)
O7W—H13W⋯N1iv 0.82 (3) 2.19 (2) 2.902 (7) 145 (3)
O7W—H14W⋯N5ii 0.82 (1) 2.37 (4) 2.758 (7) 110 (3)
O7W—H14W⋯O3W 0.82 (1) 2.29 (1) 2.709 (6) 112 (3)
O8W—H16W⋯N11v 0.82 (3) 1.98 (3) 2.798 (9) 176 (6)
O9W—H17W⋯O20 0.82 (3) 2.06 (4) 2.873 (7) 169 (6)
O9W—H18W⋯O2vi 0.82 (4) 2.24 (5) 3.028 (7) 161 (7)
N1—H1A⋯O6vi 0.86 2.22 2.972 (7) 146
N1—H1B⋯O2vi 0.86 2.14 2.958 (6) 159
N7—H7B⋯O14vii 0.86 2.51 3.289 (12) 151
N7—H7A⋯O15viii 0.86 2.63 3.345 (12) 141
N7—H7A⋯O16viii 0.86 2.46 3.302 (13) 167
Symmetry codes: (i) [-x+{\script{3\over 2}}, y-{\script{1\over 2}}, z]; (ii) x, y, z-1; (iii) -x+2, -y+1, z; (iv) [-x+2, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]; (v) [-x+{\script{3\over 2}}, y, z-{\script{1\over 2}}]; (vi) [-x+2, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]; (vii) [x, y+{\script{1\over 2}}, z+{\script{1\over 2}}]; (viii) [-x+{\script{3\over 2}}, y+{\script{1\over 2}}, z].

Data collection: APEX2 (Bruker, 2004[Bruker (2004). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2001[Bruker (2001). SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; 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.

Supporting information


Comment top

The design and synthesis of metal-organic compounds has attracted continuous research interest not only because of their appealing structural and topological novelties, but also due to their interesting optical, electronic, magnetic, and catalytic properties, as well as their potential medical applications (Karthikeyan et al., 1989). Here, we describe the synthesis and structural characterization of the title compound.

As shown in Figure 1, Gd(III) is octacoordinated by senven water molecules and one p-amino-benzenesulfonate anion. The Gd—O bond lengths are in the range of 2.370 (4)—2.439 (4) Å. In the molecule, one p-amino-benzenesulfonate, one nitrate, and two water molecules disassociate. N—H···O2, N—H···S, O—H···N, O—H···N, O—H···O hydrogen bonding between the cationic and anionic moieties and the uncoordinated water molecules leads to a consolidation of the structure (Fig. 2; Table 2).

Related literature top

For background to lanthanide coordination networks, see Karthikeyan et al. (1989).

Experimental top

A mixture of 4-aminobenzene sulfonic acid (1 mmol 0.17 g), gadolinium(III) nitrate hexahydrate (0.5 mmol, 0.17 g), and 4,4-bipyridine (1 mmol, 0.14 g) in 10 ml distilled water was sealed in a 25 ml Teflon-lined stainless steel autoclave and was kept at 433 K for three days. Colourless blocks of (I) were obtained upon cooling. Anal. C52H62GdN11O18S2: C, 46.22; H, 4.59; N, 11.41. Found: C, 46.01; H, 4.48; N, 11.23%.

Refinement top

All hydrogen atoms bound to aromatic carbon atoms were refined in calculated positions using a riding model with a C—H distance of 0.93 Å and Uiso = 1.2Ueq(C). The hydrogen atoms bound to N atoms were refined in calculated positions using a riding model with a N—H distance of 0.86 Å and Uiso = 1.2Ueq(C). Water molecules are refined by using the 'DFIX' command with the hydrogen atoms were separated with 1.38 Å, and the lengths of bond H—O were constrained with 0.82 Å with error 0.02 and Uiso = 1.5Ueq (O). The location of the water H atoms should be regarded as less certain that those of the other H atoms.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); 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).

Figures top
[Figure 1] Fig. 1. The building blocks of (I) with displacement ellipsoids drawn at the 30% probability level; H atoms are given as spheres of arbitrary radius.
[Figure 2] Fig. 2. The crystal packing of (I), displayed with N—H···O and O—H···O hydrogen bonds as dashed lines.
(4-Aminobenzenesulfonato)heptaaquagadolinium(III) 4-aminobenzenesulfonate nitrate 4,4'-bipyridyl tetrasolvate dihydrate top
Crystal data top
[Gd(C6H6O3S)(H2O)7](C6H6O3S)(NO3)·4C10H8N2·2H2OF(000) = 5528
Mr = 1350.50Dx = 1.508 Mg m3
Orthorhombic, Aba2Mo Kα radiation, λ = 0.71073 Å
Hall symbol: A 2 -2acCell parameters from 10477 reflections
a = 33.529 (2) Åθ = 2.4–25.0°
b = 23.3375 (10) ŵ = 1.26 mm1
c = 15.2046 (10) ÅT = 296 K
V = 11897.3 (12) Å3Block, colourless
Z = 80.12 × 0.10 × 0.08 mm
Data collection top
Bruker APEXII CCD
diffractometer
10477 independent reflections
Radiation source: fine-focus sealed tube8881 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.045
phi and ω scansθmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 3939
Tmin = 0.863, Tmax = 0.906k = 2725
41191 measured reflectionsl = 1818
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.036H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.088 w = 1/[σ2(Fo2) + (0.044P)2 + 12.9607P]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
10477 reflectionsΔρmax = 0.35 e Å3
811 parametersΔρmin = 0.53 e Å3
27 restraintsAbsolute structure: Flack (1983), 5009 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.002 (1)
Crystal data top
[Gd(C6H6O3S)(H2O)7](C6H6O3S)(NO3)·4C10H8N2·2H2OV = 11897.3 (12) Å3
Mr = 1350.50Z = 8
Orthorhombic, Aba2Mo Kα radiation
a = 33.529 (2) ŵ = 1.26 mm1
b = 23.3375 (10) ÅT = 296 K
c = 15.2046 (10) Å0.12 × 0.10 × 0.08 mm
Data collection top
Bruker APEXII CCD
diffractometer
10477 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
8881 reflections with I > 2σ(I)
Tmin = 0.863, Tmax = 0.906Rint = 0.045
41191 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.036H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.088 w = 1/[σ2(Fo2) + (0.044P)2 + 12.9607P]
where P = (Fo2 + 2Fc2)/3
S = 1.00Δρmax = 0.35 e Å3
10477 reflectionsΔρmin = 0.53 e Å3
811 parametersAbsolute structure: Flack (1983), 5009 Friedel pairs
27 restraintsAbsolute structure parameter: 0.002 (1)
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
C11.01881 (15)0.6735 (2)0.4126 (3)0.0317 (11)
C21.04516 (16)0.6502 (2)0.4716 (3)0.0373 (12)
H21.06130.61980.45450.045*
C31.04792 (18)0.6714 (3)0.5561 (4)0.0423 (14)
H31.06580.65490.59550.051*
C41.02425 (16)0.7174 (2)0.5830 (3)0.0366 (13)
C50.99778 (17)0.7407 (2)0.5226 (3)0.0391 (14)
H50.98180.77140.53910.047*
C60.99492 (16)0.7190 (2)0.4389 (4)0.0392 (13)
H60.97680.73500.39950.047*
C70.9597 (2)0.5837 (3)0.5639 (5)0.065 (2)
H70.96680.61490.52940.078*
C80.9629 (2)0.5891 (3)0.6540 (5)0.058 (2)
H80.97260.62300.67810.069*
C90.9520 (2)0.5445 (3)0.7085 (4)0.0402 (16)
C100.9388 (3)0.4959 (3)0.6658 (4)0.069 (2)
H100.93160.46380.69830.083*
C110.9361 (3)0.4947 (4)0.5753 (5)0.083 (3)
H110.92590.46180.54920.099*
C120.95518 (19)0.5476 (3)0.8045 (4)0.0364 (15)
C130.9811 (2)0.5832 (3)0.8464 (5)0.065 (2)
H130.99760.60720.81390.077*
C140.9829 (3)0.5837 (4)0.9365 (5)0.077 (3)
H141.00100.60840.96300.092*
C150.9355 (3)0.5184 (4)0.9479 (5)0.074 (3)
H150.91950.49500.98260.089*
C160.9307 (2)0.5152 (3)0.8572 (5)0.063 (2)
H160.91140.49150.83270.075*
C170.8646 (2)0.6318 (3)0.9382 (5)0.056 (2)
H170.85040.60590.97260.067*
C180.8591 (2)0.6306 (3)0.8485 (5)0.053 (2)
H180.84140.60420.82450.064*
C190.87929 (19)0.6675 (3)0.7936 (4)0.0357 (16)
C200.9046 (2)0.7060 (3)0.8358 (5)0.055 (2)
H200.91890.73290.80360.066*
C210.9079 (2)0.7037 (4)0.9264 (5)0.063 (2)
H210.92500.73000.95290.076*
C220.87594 (19)0.6666 (3)0.6959 (5)0.0395 (17)
C230.8567 (2)0.6225 (3)0.6532 (4)0.056 (2)
H230.84450.59330.68500.067*
C240.8556 (3)0.6222 (4)0.5622 (6)0.068 (2)
H240.84280.59180.53450.081*
C250.8918 (2)0.7093 (3)0.6430 (5)0.0504 (18)
H250.90440.74070.66850.060*
C260.8890 (2)0.7054 (3)0.5529 (5)0.058 (2)
H260.90000.73470.51910.070*
C270.7098 (2)0.7503 (4)0.9084 (5)0.077 (2)
H270.68250.75510.90030.092*
C280.7333 (2)0.7988 (3)0.9122 (5)0.066 (2)
H280.72200.83490.90620.079*
C290.77372 (19)0.7930 (3)0.9250 (4)0.0522 (16)
C300.7882 (2)0.7383 (3)0.9354 (5)0.069 (2)
H300.81530.73220.94540.083*
C310.7622 (2)0.6925 (3)0.9310 (6)0.083 (3)
H310.77250.65590.93960.099*
C320.80115 (18)0.8427 (3)0.9256 (4)0.0506 (15)
C330.7922 (2)0.8937 (3)0.9665 (5)0.072 (2)
H330.76830.89830.99690.087*
C340.8197 (3)0.9385 (3)0.9614 (6)0.078 (2)
H340.81350.97250.99030.094*
C350.8615 (2)0.8864 (3)0.8783 (5)0.0587 (18)
H350.88510.88360.84640.070*
C360.8371 (2)0.8394 (3)0.8811 (5)0.0566 (18)
H360.84460.80550.85340.068*
C370.7417 (2)0.7246 (3)0.1777 (6)0.071 (2)
H370.71480.71510.18140.086*
C380.7696 (2)0.6819 (3)0.1772 (6)0.081 (2)
H380.76090.64420.18050.097*
C390.8195 (2)0.7462 (4)0.1683 (5)0.072 (2)
H390.84660.75420.16540.087*
C400.79343 (19)0.7909 (3)0.1685 (5)0.0617 (18)
H400.80310.82820.16550.074*
C410.75276 (18)0.7816 (3)0.1729 (4)0.0501 (15)
C420.72368 (16)0.8286 (3)0.1737 (4)0.0444 (14)
C430.68574 (18)0.8222 (3)0.1372 (4)0.0564 (17)
H430.67840.78810.11010.068*
C440.6595 (2)0.8671 (4)0.1419 (5)0.063 (2)
H440.63440.86200.11700.075*
C450.73194 (17)0.8813 (3)0.2124 (4)0.0541 (17)
H450.75680.88810.23760.065*
C460.7029 (2)0.9237 (3)0.2131 (5)0.063 (2)
H460.70900.95870.23890.075*
C470.87083 (17)0.8856 (2)0.3376 (4)0.0432 (14)
C480.86031 (16)0.9022 (2)0.2554 (6)0.0486 (14)
H480.87210.88450.20720.058*
C490.83240 (17)0.9449 (3)0.2418 (7)0.0632 (16)
H490.82560.95520.18470.076*
C500.81468 (18)0.9721 (3)0.3113 (6)0.0602 (18)
C510.8256 (2)0.9552 (3)0.3948 (5)0.0631 (19)
H510.81400.97300.44320.076*
C520.8533 (2)0.9124 (3)0.4081 (4)0.0557 (17)
H520.86020.90160.46500.067*
Gd10.914673 (6)0.583155 (8)0.24786 (4)0.02827 (7)
N11.02869 (15)0.7404 (2)0.6662 (3)0.0519 (13)
H1A1.04610.72640.70170.062*
H1B1.01400.76870.68240.062*
N20.7594 (2)0.5425 (3)0.0739 (6)0.0738 (19)
N30.9470 (2)0.5368 (3)0.5235 (4)0.0637 (19)
N40.9609 (2)0.5518 (3)0.9875 (4)0.0626 (17)
N50.88924 (17)0.6679 (3)0.9780 (4)0.0525 (15)
N60.87160 (17)0.6623 (3)0.5119 (4)0.0558 (15)
N70.78776 (18)1.0158 (3)0.2970 (5)0.088 (2)
H7A0.78201.02620.24420.106*
H7B0.77671.03280.34090.106*
N80.80819 (19)0.6914 (3)0.1722 (5)0.0732 (17)
N90.66714 (17)0.9169 (2)0.1790 (4)0.0606 (14)
N100.8535 (2)0.9358 (3)0.9186 (5)0.0723 (17)
N110.72363 (19)0.6974 (3)0.9154 (5)0.0815 (19)
O10.97175 (11)0.64181 (16)0.2889 (3)0.0445 (9)
O21.03318 (10)0.68583 (14)0.2462 (4)0.0483 (8)
O31.03391 (12)0.59050 (16)0.3044 (3)0.0515 (10)
O50.88950 (15)0.77808 (18)0.3359 (4)0.0797 (16)
O60.93894 (13)0.84568 (19)0.2913 (3)0.0678 (13)
O140.7721 (3)0.5527 (4)0.0030 (7)0.185 (5)
O150.7793 (2)0.5406 (3)0.1387 (7)0.155 (4)
O160.7249 (2)0.5362 (4)0.0840 (6)0.143 (3)
O200.92070 (18)0.8376 (2)0.4442 (3)0.0874 (17)
O1W0.88775 (12)0.65990 (17)0.3333 (2)0.0464 (10)
O2W0.86855 (12)0.54534 (19)0.3511 (3)0.0533 (11)
O3W0.85363 (11)0.59444 (18)0.1683 (3)0.0483 (10)
O4W0.89860 (12)0.49138 (17)0.1797 (3)0.0485 (10)
O5W0.96918 (11)0.54819 (17)0.1606 (2)0.0418 (9)
O6W0.95002 (14)0.52250 (18)0.3461 (2)0.0468 (10)
O7W0.91889 (12)0.66144 (19)0.1469 (3)0.0490 (11)
O8W0.7948 (2)0.5832 (3)0.3771 (5)0.0923 (19)
O9W0.94198 (16)0.8969 (2)0.6030 (3)0.0660 (13)
S21.01437 (4)0.64533 (6)0.30545 (9)0.0351 (3)
S50.90793 (5)0.83258 (7)0.35428 (12)0.0509 (4)
H1W0.8955 (12)0.6538 (11)0.3835 (6)0.076*
H2W0.8968 (11)0.68906 (11)0.3108 (18)0.076*
H3W0.8467 (2)0.5584 (15)0.3374 (17)0.076*
H6W0.8437 (6)0.6238 (9)0.1882 (18)0.076*
H8W0.8762 (5)0.4857 (9)0.199 (2)0.076*
H9W0.9625 (6)0.5555 (17)0.1100 (2)0.076*
H10W0.9884 (2)0.5665 (14)0.178 (2)0.076*
H11W0.955 (2)0.4895 (9)0.331 (3)0.076*
H12W0.950 (2)0.527 (2)0.3995 (6)0.076*
H14W0.89570 (17)0.6682 (13)0.133 (2)0.076*
H16W0.789 (2)0.6161 (9)0.390 (4)0.076*
H17W0.937 (2)0.884 (2)0.5539 (16)0.076*
H18W0.943 (2)0.8730 (18)0.642 (3)0.076*
H15W0.793 (2)0.5599 (18)0.417 (3)0.06 (3)*
H5W0.8410 (5)0.5651 (7)0.179 (2)0.14 (4)*
H4W0.8703 (9)0.51038 (19)0.347 (2)0.22 (7)*
H7W0.9160 (8)0.4709 (4)0.201 (2)0.15 (5)*
H13W0.9299 (13)0.6871 (7)0.1746 (11)0.15 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.031 (3)0.034 (3)0.030 (3)0.004 (2)0.001 (2)0.001 (2)
C20.038 (3)0.038 (3)0.036 (3)0.010 (2)0.001 (2)0.000 (2)
C30.044 (3)0.049 (4)0.034 (3)0.001 (3)0.014 (3)0.003 (3)
C40.039 (3)0.038 (3)0.033 (3)0.006 (3)0.003 (2)0.004 (2)
C50.040 (3)0.036 (3)0.041 (4)0.006 (3)0.001 (3)0.009 (3)
C60.038 (3)0.038 (3)0.042 (3)0.005 (2)0.005 (2)0.000 (3)
C70.062 (5)0.076 (6)0.057 (5)0.003 (4)0.009 (4)0.022 (4)
C80.064 (5)0.069 (5)0.040 (4)0.021 (4)0.001 (4)0.001 (4)
C90.041 (4)0.040 (4)0.039 (3)0.002 (3)0.009 (3)0.005 (3)
C100.124 (7)0.049 (5)0.035 (4)0.016 (4)0.002 (4)0.003 (3)
C110.142 (8)0.058 (5)0.049 (5)0.013 (5)0.007 (5)0.005 (4)
C120.038 (3)0.045 (4)0.027 (3)0.005 (3)0.001 (3)0.001 (3)
C130.063 (5)0.080 (6)0.051 (4)0.030 (4)0.003 (4)0.008 (4)
C140.072 (5)0.108 (7)0.050 (5)0.028 (5)0.012 (4)0.021 (5)
C150.110 (7)0.078 (7)0.034 (5)0.015 (5)0.009 (4)0.001 (4)
C160.075 (5)0.072 (5)0.041 (4)0.029 (4)0.006 (4)0.006 (4)
C170.070 (5)0.057 (5)0.041 (4)0.012 (4)0.001 (3)0.017 (4)
C180.056 (4)0.047 (4)0.057 (5)0.019 (4)0.011 (4)0.001 (4)
C190.041 (4)0.038 (4)0.029 (3)0.001 (3)0.008 (3)0.006 (3)
C200.058 (4)0.067 (5)0.041 (4)0.024 (4)0.000 (3)0.010 (3)
C210.070 (5)0.073 (5)0.047 (4)0.027 (4)0.018 (4)0.003 (4)
C220.036 (4)0.040 (4)0.042 (4)0.011 (3)0.003 (3)0.001 (4)
C230.080 (5)0.060 (5)0.028 (4)0.022 (4)0.002 (3)0.001 (3)
C240.081 (6)0.071 (6)0.051 (5)0.028 (5)0.003 (4)0.009 (4)
C250.066 (5)0.043 (4)0.042 (4)0.010 (3)0.000 (3)0.004 (3)
C260.075 (5)0.055 (5)0.045 (4)0.002 (4)0.006 (4)0.011 (4)
C270.044 (4)0.108 (7)0.078 (5)0.015 (5)0.005 (4)0.012 (5)
C280.048 (4)0.067 (5)0.081 (5)0.006 (4)0.008 (4)0.019 (4)
C290.051 (4)0.048 (4)0.057 (4)0.003 (3)0.004 (3)0.004 (3)
C300.050 (4)0.054 (4)0.103 (6)0.007 (3)0.016 (4)0.012 (4)
C310.067 (5)0.057 (5)0.123 (8)0.014 (4)0.013 (5)0.013 (5)
C320.047 (4)0.047 (4)0.058 (4)0.000 (3)0.001 (3)0.018 (3)
C330.080 (5)0.052 (4)0.085 (6)0.005 (4)0.028 (4)0.007 (4)
C340.106 (6)0.047 (4)0.081 (5)0.002 (4)0.017 (5)0.003 (4)
C350.051 (4)0.059 (5)0.066 (5)0.005 (4)0.004 (3)0.013 (4)
C360.047 (4)0.047 (4)0.075 (5)0.004 (3)0.012 (3)0.002 (4)
C370.045 (4)0.060 (5)0.109 (6)0.004 (3)0.004 (4)0.007 (4)
C380.068 (5)0.055 (5)0.119 (7)0.010 (4)0.010 (5)0.010 (5)
C390.042 (4)0.086 (6)0.089 (6)0.006 (4)0.010 (4)0.014 (5)
C400.046 (4)0.049 (4)0.090 (5)0.006 (3)0.017 (4)0.001 (4)
C410.046 (4)0.054 (4)0.050 (4)0.001 (3)0.007 (3)0.006 (3)
C420.039 (3)0.053 (4)0.041 (3)0.002 (3)0.005 (3)0.003 (3)
C430.044 (4)0.065 (5)0.061 (4)0.007 (3)0.006 (3)0.008 (3)
C440.041 (4)0.078 (6)0.069 (5)0.008 (4)0.008 (3)0.008 (4)
C450.041 (3)0.049 (4)0.073 (4)0.005 (3)0.002 (3)0.006 (3)
C460.058 (4)0.045 (4)0.084 (5)0.005 (3)0.001 (3)0.001 (3)
C470.047 (3)0.036 (3)0.047 (4)0.008 (3)0.006 (3)0.000 (3)
C480.055 (3)0.046 (3)0.045 (3)0.005 (2)0.001 (4)0.003 (4)
C490.060 (3)0.057 (4)0.073 (4)0.001 (3)0.016 (5)0.008 (5)
C500.040 (3)0.041 (4)0.099 (6)0.007 (3)0.002 (4)0.012 (4)
C510.061 (4)0.058 (5)0.070 (5)0.004 (4)0.017 (4)0.009 (4)
C520.059 (4)0.058 (4)0.049 (4)0.006 (3)0.012 (3)0.007 (3)
Gd10.03323 (11)0.02543 (11)0.02617 (10)0.00137 (9)0.00040 (18)0.00023 (17)
N10.067 (3)0.053 (3)0.036 (3)0.003 (3)0.008 (2)0.011 (2)
N20.064 (4)0.056 (4)0.101 (6)0.008 (3)0.026 (4)0.001 (4)
N30.093 (5)0.069 (5)0.028 (3)0.011 (4)0.002 (3)0.005 (3)
N40.069 (4)0.077 (5)0.042 (3)0.011 (3)0.006 (3)0.008 (3)
N50.056 (3)0.058 (4)0.043 (3)0.007 (3)0.009 (3)0.011 (3)
N60.063 (4)0.070 (4)0.035 (3)0.005 (3)0.004 (3)0.006 (3)
N70.078 (4)0.063 (4)0.124 (6)0.023 (4)0.013 (4)0.020 (4)
N80.065 (4)0.067 (4)0.087 (5)0.022 (3)0.015 (3)0.005 (4)
N90.059 (4)0.056 (4)0.067 (4)0.010 (3)0.003 (3)0.008 (3)
N100.081 (4)0.055 (4)0.081 (4)0.014 (3)0.009 (4)0.010 (3)
N110.064 (4)0.076 (5)0.104 (5)0.019 (4)0.007 (4)0.011 (4)
O10.042 (2)0.044 (2)0.047 (2)0.0058 (18)0.0118 (17)0.0100 (18)
O20.056 (2)0.052 (2)0.0373 (17)0.0096 (16)0.003 (3)0.003 (3)
O30.063 (3)0.041 (2)0.051 (2)0.012 (2)0.000 (2)0.0114 (19)
O50.081 (3)0.033 (3)0.125 (5)0.003 (2)0.007 (3)0.002 (3)
O60.054 (3)0.068 (3)0.082 (3)0.004 (2)0.013 (2)0.004 (3)
O140.277 (14)0.140 (7)0.136 (7)0.073 (7)0.105 (9)0.027 (7)
O150.138 (6)0.094 (5)0.232 (10)0.034 (5)0.109 (7)0.059 (6)
O160.073 (5)0.174 (8)0.181 (8)0.017 (5)0.017 (5)0.019 (7)
O200.109 (5)0.089 (4)0.064 (3)0.024 (3)0.029 (3)0.009 (3)
O1W0.069 (3)0.039 (2)0.031 (2)0.001 (2)0.010 (2)0.0043 (17)
O2W0.053 (3)0.041 (3)0.066 (3)0.004 (2)0.020 (2)0.015 (2)
O3W0.039 (2)0.036 (2)0.070 (3)0.0021 (19)0.010 (2)0.000 (2)
O4W0.040 (2)0.039 (2)0.066 (3)0.002 (2)0.005 (2)0.010 (2)
O5W0.038 (2)0.052 (3)0.036 (2)0.0039 (19)0.0014 (17)0.0115 (19)
O6W0.066 (3)0.046 (3)0.028 (2)0.010 (2)0.002 (2)0.0045 (18)
O7W0.055 (3)0.052 (3)0.040 (2)0.012 (2)0.017 (2)0.016 (2)
O8W0.078 (4)0.086 (5)0.113 (5)0.030 (4)0.004 (4)0.014 (5)
O9W0.078 (3)0.069 (3)0.052 (3)0.009 (3)0.004 (3)0.004 (2)
S20.0392 (7)0.0337 (7)0.0324 (7)0.0002 (6)0.0037 (6)0.0052 (6)
S50.0543 (9)0.0388 (9)0.0594 (10)0.0008 (7)0.0002 (8)0.0030 (7)
Geometric parameters (Å, º) top
C1—C21.371 (7)C35—H350.9300
C1—C61.389 (7)C36—H360.9300
C1—S21.763 (5)C37—C381.367 (9)
C2—C31.380 (8)C37—C411.384 (9)
C2—H20.9300C37—H370.9300
C3—C41.396 (8)C38—N81.314 (9)
C3—H30.9300C38—H380.9300
C4—N11.382 (7)C39—N81.335 (9)
C4—C51.388 (8)C39—C401.361 (9)
C5—C61.372 (8)C39—H390.9300
C5—H50.9300C40—C411.382 (9)
C6—H60.9300C40—H400.9300
C7—N31.324 (10)C41—C421.468 (8)
C7—C81.380 (11)C42—C431.396 (8)
C7—H70.9300C42—C451.391 (8)
C8—C91.380 (9)C43—C441.369 (9)
C8—H80.9300C43—H430.9300
C9—C101.380 (10)C44—N91.317 (9)
C9—C121.465 (8)C44—H440.9300
C10—C111.379 (10)C45—C461.389 (9)
C10—H100.9300C45—H450.9300
C11—N31.312 (10)C46—N91.316 (9)
C11—H110.9300C46—H460.9300
C12—C131.361 (9)C47—C481.355 (10)
C12—C161.373 (9)C47—C521.372 (8)
C13—C141.372 (11)C47—S51.773 (6)
C13—H130.9300C48—C491.382 (8)
C14—N41.302 (10)C48—H480.9300
C14—H140.9300C49—C501.369 (11)
C15—N41.302 (10)C49—H490.9300
C15—C161.391 (10)C50—N71.381 (8)
C15—H150.9300C50—C511.378 (10)
C16—H160.9300C51—C521.381 (10)
C17—N51.325 (9)C51—H510.9300
C17—C181.376 (10)C52—H520.9300
C17—H170.9300Gd1—O6W2.375 (4)
C18—C191.377 (9)Gd1—O2W2.373 (4)
C18—H180.9300Gd1—O1W2.389 (4)
C19—C201.392 (9)Gd1—O3W2.392 (4)
C19—C221.489 (6)Gd1—O7W2.391 (4)
C20—C211.383 (10)Gd1—O5W2.401 (4)
C20—H200.9300Gd1—O12.434 (4)
C21—N51.307 (9)Gd1—O4W2.440 (4)
C21—H210.9300N1—H1A0.8600
C22—C251.388 (9)N1—H1B0.8600
C22—C231.377 (9)N2—O161.176 (8)
C23—C241.384 (10)N2—O141.184 (10)
C23—H230.9300N2—O151.190 (9)
C24—N61.322 (10)N7—H7A0.8600
C24—H240.9300N7—H7B0.8600
C25—C261.376 (9)O1—S21.453 (4)
C25—H250.9300O2—S21.450 (4)
C26—N61.320 (9)O3—S21.438 (4)
C26—H260.9300O5—S51.441 (5)
C27—N111.322 (10)O6—S51.446 (5)
C27—C281.381 (10)O20—S51.437 (5)
C27—H270.9300O1W—H1W0.819 (17)
C28—C291.375 (9)O1W—H2W0.820 (19)
C28—H280.9300O2W—H3W0.820 (17)
C29—C301.376 (9)O2W—H4W0.820 (7)
C29—C321.481 (9)O3W—H6W0.82 (2)
C30—C311.380 (10)O3W—H5W0.821 (18)
C30—H300.9300O4W—H8W0.82 (2)
C31—N111.321 (9)O4W—H7W0.82 (2)
C31—H310.9300O5W—H9W0.819 (11)
C32—C361.385 (9)O5W—H10W0.82 (2)
C32—C331.377 (10)O6W—H11W0.82 (3)
C33—C341.395 (10)O6W—H12W0.819 (12)
C33—H330.9300O8W—H16W0.82 (3)
C34—N101.310 (10)O8W—H15W0.82 (4)
C34—H340.9300O9W—H17W0.82 (3)
C35—N101.335 (9)O9W—H18W0.82 (4)
C35—C361.369 (9)
C2—C1—C6119.1 (5)C39—C40—C41120.9 (7)
C2—C1—S2120.7 (4)C39—C40—H40119.5
C6—C1—S2120.2 (4)C41—C40—H40119.5
C1—C2—C3120.6 (5)C37—C41—C40114.7 (6)
C1—C2—H2119.7C37—C41—C42122.7 (6)
C3—C2—H2119.7C40—C41—C42122.6 (6)
C2—C3—C4120.7 (5)C43—C42—C45116.4 (6)
C2—C3—H3119.6C43—C42—C41121.5 (6)
C4—C3—H3119.6C45—C42—C41122.1 (5)
N1—C4—C3120.4 (5)C44—C43—C42118.8 (7)
N1—C4—C5121.5 (5)C44—C43—H43120.6
C3—C4—C5118.1 (5)C42—C43—H43120.6
C6—C5—C4120.9 (5)N9—C44—C43125.0 (7)
C6—C5—H5119.5N9—C44—H44117.5
C4—C5—H5119.5C43—C44—H44117.5
C5—C6—C1120.5 (5)C46—C45—C42119.6 (6)
C5—C6—H6119.7C46—C45—H45120.2
C1—C6—H6119.7C42—C45—H45120.2
N3—C7—C8124.3 (7)N9—C46—C45123.3 (7)
N3—C7—H7117.9N9—C46—H46118.3
C8—C7—H7117.9C45—C46—H46118.3
C7—C8—C9120.4 (7)C48—C47—C52118.6 (6)
C7—C8—H8119.8C48—C47—S5120.9 (5)
C9—C8—H8119.8C52—C47—S5120.4 (5)
C8—C9—C10115.0 (6)C47—C48—C49121.3 (8)
C8—C9—C12122.8 (7)C47—C48—H48119.3
C10—C9—C12122.2 (7)C49—C48—H48119.3
C11—C10—C9120.5 (7)C50—C49—C48120.9 (9)
C11—C10—H10119.8C50—C49—H49119.6
C9—C10—H10119.8C48—C49—H49119.6
N3—C11—C10124.4 (8)C49—C50—N7120.4 (8)
N3—C11—H11117.8C49—C50—C51117.6 (7)
C10—C11—H11117.8N7—C50—C51122.0 (7)
C13—C12—C16116.4 (6)C52—C51—C50121.3 (7)
C13—C12—C9122.8 (7)C52—C51—H51119.3
C16—C12—C9120.7 (7)C50—C51—H51119.3
C12—C13—C14120.0 (7)C51—C52—C47120.2 (6)
C12—C13—H13120.0C51—C52—H52119.9
C14—C13—H13120.0C47—C52—H52119.9
N4—C14—C13124.5 (7)O6W—Gd1—O2W71.80 (15)
N4—C14—H14117.8O6W—Gd1—O1W107.07 (14)
C13—C14—H14117.8O2W—Gd1—O1W70.93 (15)
N4—C15—C16124.5 (8)O6W—Gd1—O3W144.17 (16)
N4—C15—H15117.7O2W—Gd1—O3W79.51 (15)
C16—C15—H15117.7O1W—Gd1—O3W82.48 (14)
C12—C16—C15118.6 (7)O6W—Gd1—O7W146.10 (15)
C12—C16—H16120.7O2W—Gd1—O7W138.36 (14)
C15—C16—H16120.7O1W—Gd1—O7W78.38 (14)
N5—C17—C18123.2 (7)O3W—Gd1—O7W68.99 (14)
N5—C17—H17118.4O6W—Gd1—O5W76.42 (13)
C18—C17—H17118.4O2W—Gd1—O5W137.30 (14)
C17—C18—C19121.5 (7)O1W—Gd1—O5W147.41 (14)
C17—C18—H18119.2O3W—Gd1—O5W114.14 (14)
C19—C18—H18119.2O7W—Gd1—O5W81.94 (14)
C20—C19—C18115.0 (6)O6W—Gd1—O177.38 (15)
C20—C19—C22121.0 (7)O2W—Gd1—O1123.49 (14)
C18—C19—C22124.0 (7)O1W—Gd1—O174.70 (13)
C21—C20—C19118.9 (7)O3W—Gd1—O1137.76 (14)
C21—C20—H20120.5O7W—Gd1—O171.85 (14)
C19—C20—H20120.5O5W—Gd1—O174.60 (13)
N5—C21—C20125.7 (7)O6W—Gd1—O4W81.63 (15)
N5—C21—H21117.2O2W—Gd1—O4W79.08 (15)
C20—C21—H21117.1O1W—Gd1—O4W143.66 (14)
C25—C22—C23116.3 (7)O3W—Gd1—O4W72.10 (15)
C25—C22—C19122.6 (7)O7W—Gd1—O4W114.26 (15)
C23—C22—C19121.1 (7)O5W—Gd1—O4W68.59 (13)
C24—C23—C22119.1 (7)O1—Gd1—O4W140.92 (13)
C24—C23—H23120.4C4—N1—H1A120.0
C22—C23—H23120.4C4—N1—H1B120.0
N6—C24—C23124.4 (8)H1A—N1—H1B120.0
N6—C24—H24117.8O16—N2—O14119.8 (10)
C23—C24—H24117.8O16—N2—O15116.1 (10)
C22—C25—C26120.2 (7)O14—N2—O15124.0 (10)
C22—C25—H25119.9C7—N3—C11115.4 (7)
C26—C25—H25119.9C14—N4—C15115.8 (7)
N6—C26—C25123.4 (7)C21—N5—C17115.6 (6)
N6—C26—H26118.3C26—N6—C24116.5 (6)
C25—C26—H26118.3C50—N7—H7A120.0
N11—C27—C28124.1 (7)C50—N7—H7B120.0
N11—C27—H27118.0H7A—N7—H7B120.0
C28—C27—H27118.0C38—N8—C39116.3 (6)
C29—C28—C27119.2 (7)C38—N8—H14W158.5 (9)
C29—C28—H28120.4C39—N8—H14W83.6 (7)
C27—C28—H28120.4C46—N9—C44116.9 (6)
C30—C29—C28117.1 (6)C34—N10—C35116.3 (7)
C30—C29—C32120.5 (6)C27—N11—C31116.1 (7)
C28—C29—C32122.4 (6)S2—O1—Gd1148.1 (2)
C31—C30—C29119.3 (7)S2—O2—H13W77.1 (2)
C31—C30—H30120.4Gd1—O1W—H1W105 (2)
C29—C30—H30120.4Gd1—O1W—H2W104.8 (18)
N11—C31—C30124.1 (8)H1W—O1W—H2W115 (3)
N11—C31—H31118.0Gd1—O2W—H3W106.0 (19)
C30—C31—H31118.0Gd1—O2W—H4W106 (2)
C36—C32—C33117.4 (6)H3W—O2W—H4W115 (3)
C36—C32—C29119.6 (6)Gd1—O3W—H6W104.7 (17)
C33—C32—C29123.0 (6)Gd1—O3W—H5W104.4 (16)
C32—C33—C34118.5 (7)H6W—O3W—H5W115 (2)
C32—C33—H33120.7Gd1—O4W—H8W101.1 (17)
C34—C33—H33120.7Gd1—O4W—H7W100.8 (14)
N10—C34—C33124.4 (8)H8W—O4W—H7W115 (3)
N10—C34—H34117.8Gd1—O5W—H9W103.9 (17)
C33—C34—H34117.8Gd1—O5W—H10W104.1 (18)
N10—C35—C36124.0 (7)H9W—O5W—H10W114 (3)
N10—C35—H35118.0Gd1—O6W—H11W118 (4)
C36—C35—H35118.0Gd1—O6W—H12W122 (4)
C35—C36—C32119.4 (7)H11W—O6W—H12W114 (5)
C35—C36—H36120.3H16W—O8W—H15W116 (5)
C32—C36—H36120.3H17W—O9W—H18W115 (4)
C38—C37—C41121.1 (7)O3—S2—O2112.1 (2)
C38—C37—H37119.4O3—S2—O1113.3 (2)
C41—C37—H37119.4O2—S2—O1110.9 (2)
N8—C38—C37123.5 (7)O3—S2—C1107.7 (2)
N8—C38—H38118.3O2—S2—C1107.1 (3)
C37—C38—H38118.3O1—S2—C1105.3 (2)
N8—C39—C40123.5 (7)O20—S5—O6113.5 (3)
N8—C39—H39118.3O20—S5—O5112.6 (4)
C40—C39—H39118.3O6—S5—O5111.5 (3)
N8—C39—H14W71.8 (5)O20—S5—C47106.7 (3)
C40—C39—H14W162.6 (6)O6—S5—C47105.2 (3)
H39—C39—H14W47.3O5—S5—C47106.7 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···N60.82 (2)2.12 (2)2.770 (7)136 (3)
O1W—H2W···O50.82 (2)2.13 (1)2.759 (6)134 (3)
O2W—H3W···O8W0.82 (2)1.93 (1)2.657 (7)147 (2)
O3W—H6W···N80.82 (2)1.99 (1)2.728 (7)149 (2)
O4W—H8W···N9i0.82 (2)2.19 (2)2.807 (7)133 (1)
O5W—H9W···N4ii0.82 (1)1.86 (1)2.647 (7)159 (2)
O5W—H10W···O30.82 (2)2.51 (2)3.236 (6)148 (4)
O5W—H10W···O10.82 (2)2.50 (3)2.931 (5)114 (2)
O6W—H11W···O3iii0.82 (3)1.95 (3)2.765 (6)175 (5)
O6W—H12W···N30.82 (1)1.90 (1)2.719 (7)178 (8)
O7W—H13W···N1iv0.82 (3)2.19 (2)2.902 (7)145 (3)
O7W—H14W···N5ii0.82 (1)2.37 (4)2.758 (7)110 (3)
O7W—H14W···O3W0.82 (1)2.29 (1)2.709 (6)112 (3)
O8W—H16W···N11v0.82 (3)1.98 (3)2.798 (9)176 (6)
O9W—H17W···O200.82 (3)2.06 (4)2.873 (7)169 (6)
O9W—H18W···O2vi0.82 (4)2.24 (5)3.028 (7)161 (7)
N1—H1A···O6vi0.862.222.972 (7)146
N1—H1B···O2vi0.862.142.958 (6)159
N7—H7B···O14vii0.862.513.289 (12)151
N7—H7A···O15viii0.862.633.345 (12)141
N7—H7A···O16viii0.862.463.302 (13)167
Symmetry codes: (i) x+3/2, y1/2, z; (ii) x, y, z1; (iii) x+2, y+1, z; (iv) x+2, y+3/2, z1/2; (v) x+3/2, y, z1/2; (vi) x+2, y+3/2, z+1/2; (vii) x, y+1/2, z+1/2; (viii) x+3/2, y+1/2, z.

Experimental details

Crystal data
Chemical formula[Gd(C6H6O3S)(H2O)7](C6H6O3S)(NO3)·4C10H8N2·2H2O
Mr1350.50
Crystal system, space groupOrthorhombic, Aba2
Temperature (K)296
a, b, c (Å)33.529 (2), 23.3375 (10), 15.2046 (10)
V3)11897.3 (12)
Z8
Radiation typeMo Kα
µ (mm1)1.26
Crystal size (mm)0.12 × 0.10 × 0.08
Data collection
DiffractometerBruker APEXII CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.863, 0.906
No. of measured, independent and
observed [I > 2σ(I)] reflections
41191, 10477, 8881
Rint0.045
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.036, 0.088, 1.00
No. of reflections10477
No. of parameters811
No. of restraints27
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
w = 1/[σ2(Fo2) + (0.044P)2 + 12.9607P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.35, 0.53
Absolute structureFlack (1983), 5009 Friedel pairs
Absolute structure parameter0.002 (1)

Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Gd1—O6W2.375 (4)Gd1—O7W2.391 (4)
Gd1—O2W2.373 (4)Gd1—O5W2.401 (4)
Gd1—O1W2.389 (4)Gd1—O12.434 (4)
Gd1—O3W2.392 (4)Gd1—O4W2.440 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···N60.819 (17)2.12 (2)2.770 (7)136 (3)
O1W—H2W···O50.820 (19)2.127 (5)2.759 (6)134 (3)
O2W—H3W···O8W0.820 (17)1.932 (14)2.657 (7)147 (2)
O3W—H6W···N80.82 (2)1.991 (10)2.728 (7)149.2 (17)
O4W—H8W···N9i0.82 (2)2.19 (2)2.807 (7)132.5 (5)
O5W—H9W···N4ii0.819 (11)1.864 (8)2.647 (7)159.4 (16)
O5W—H10W···O30.82 (2)2.51 (2)3.236 (6)148 (4)
O5W—H10W···O10.82 (2)2.50 (3)2.931 (5)114.2 (16)
O6W—H11W···O3iii0.82 (3)1.95 (3)2.765 (6)175 (5)
O6W—H12W···N30.819 (12)1.899 (8)2.719 (7)178 (8)
O7W—H13W···N1iv0.82 (3)2.193 (16)2.902 (7)145 (3)
O7W—H14W···N5ii0.821 (12)2.37 (4)2.758 (7)110 (3)
O7W—H14W···O3W0.821 (12)2.289 (14)2.709 (6)112 (3)
O8W—H16W···N11v0.82 (3)1.98 (3)2.798 (9)176 (6)
O9W—H17W···O200.82 (3)2.06 (4)2.873 (7)169 (6)
O9W—H18W···O2vi0.82 (4)2.24 (5)3.028 (7)161 (7)
N1—H1A···O6vi0.862.222.972 (7)146
N1—H1B···O2vi0.862.142.958 (6)159
N7—H7B···O14vii0.862.513.289 (12)151
N7—H7A···O15viii0.862.633.345 (12)141
N7—H7A···O16viii0.862.463.302 (13)167
Symmetry codes: (i) x+3/2, y1/2, z; (ii) x, y, z1; (iii) x+2, y+1, z; (iv) x+2, y+3/2, z1/2; (v) x+3/2, y, z1/2; (vi) x+2, y+3/2, z+1/2; (vii) x, y+1/2, z+1/2; (viii) x+3/2, y+1/2, z.
 

Acknowledgements

Financial support from the Inter­national Cooperation Program for Excellent Lectures of 2008 by Shandong Provincial Education Department is gratefully acknowledged.

References

First citationBruker (2001). SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
First citationBruker (2004). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
First citationFlack, H. D. (1983). Acta Cryst. A39, 876–881.  CrossRef CAS Web of Science IUCr Journals
First citationKarthikeyan, S., Ryan, R. R. & Paine, R. T. (1989). Inorg. Chem. 28, 2783–2789.  CSD CrossRef CAS Web of Science
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals

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Volume 66| Part 7| July 2010| Pages m740-m741
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