Poly[[diaqua­bis­(μ3-isonicotinato-κ3N:O:O′)bis­(μ2-isonicotinato-κ2N:O)gadolinium(III)disiliver(I)] nitrate monohydrate]

Fan, L.-Q.; Wu, J.-H.

doi:10.1107/S1600536810035634

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 10| October 2010| Pages m1234-m1235

doi:10.1107/S1600536810035634

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Poly[[diaquabis(μ₃-isonicotinato-κ³N:O:O′)bis(μ₂-isonicotinato-κ²N:O)gadolinium(III)disiliver(I)] nitrate monohydrate]

Le-Qing Fan ^a ^* and Ji-Huai Wu ^a

^aInstitute of Materials Physical Chemistry, and The Key Laboratory for Functional Materials of Fujian Higher Education, Huaqiao University, Quanzhou, Fujian 362021, People's Republic of China
^*Correspondence e-mail: lqfan@hqu.edu.cn

(Received 19 August 2010; accepted 5 September 2010; online 11 September 2010)

In the title compound, {[Ag₂Gd(C₆H₄NO₂)₄(H₂O)₂]NO₃·H₂O}_n, the Gd^III ion is coordinated by eight O atoms from six isonicotinate ligands and two water molecules in a distorted square antiprismatic geometry. Two Ag^I ions are each bonded to two N atoms from two isonicotinate ligands in a linear or bow-like fashion [N—Ag—N angles = 178.6 (2) and 147.1 (2)°]. These metal ions are connected by the isonicotinate ligands into a layer parallel to (010). O—H⋯O hydrogen bonds donated by the coordinated and uncoordinated water molecules and intralayer π–π stacking interactions between the pyridine rings [centroid–centroid distances = 3.551 (4) and 3.555 (4) Å] are observed. The layers interact with each other by interlayer Ag⋯O(aqua) contacts [2.731 (4) Å] and π–π stacking interactions between the pyridine rings [centroid–centroid distances = 3.466 (3) and 3.516 (3) Å], resulting in the formation of a three-dimensional supramolecular structure.

Related literature

For general background to the structures and properties of lanthanide–transition metal coordination polymers, see: Cheng et al. (2007 , 2008 ); Fan & Wu (2010 ); Fang et al. (2009 ); Luo et al. (2007 ).

Experimental

Crystal data

[Ag₂Gd(C₆H₄NO₂)₄(H₂O)₂]NO₃·H₂O
M_r = 977.46
Monoclinic, P 2₁ /c
a = 16.889 (8) Å
b = 24.744 (11) Å
c = 6.750 (3) Å
β = 96.240 (9)°
V = 2804 (2) Å³
Z = 4
Mo Kα radiation
μ = 3.80 mm⁻¹
T = 293 K
0.30 × 0.12 × 0.08 mm

Data collection

Rigaku Mercury CCD diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2007 ) T_min = 0.703, T_max = 1.000
16445 measured reflections
4859 independent reflections
4370 reflections with I > 2σ(I)
R_int = 0.032

Refinement

R[F² > 2σ(F²)] = 0.034
wR(F²) = 0.129
S = 1.08
4859 reflections
416 parameters
H-atom parameters constrained
Δρ_max = 1.38 e Å⁻³
Δρ_min = −1.27 e Å⁻³

Table 1
Selected bond lengths (Å)

Gd1—O1	2.357 (4)
Gd1—O2ⁱ	2.465 (4)
Gd1—O3	2.383 (4)
Gd1—O5	2.393 (4)
Gd1—O7	2.399 (4)
Gd1—O8ⁱ	2.386 (4)
Gd1—O9	2.454 (4)
Gd1—O10	2.533 (4)
Ag1—N1	2.144 (5)
Ag1—N4ⁱⁱ	2.147 (5)
Ag2—N2ⁱⁱⁱ	2.189 (5)
Ag2—N3	2.199 (5)
Symmetry codes: (i) $[x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (ii) x+1, y, z; (iii) x-1, y, z.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O9—H9A⋯O6	0.85	2.13	2.771 (7)	132
O9—H9B⋯O2^iv	0.85	2.03	2.811 (6)	153
O10—H10A⋯O6^v	0.85	2.12	2.954 (6)	165
O10—H10C⋯O4	0.85	1.84	2.662 (6)	162
O14—H14B⋯O12^vi	0.85	2.27	2.960 (9)	139
O14—H14C⋯O13^vii	0.85	2.01	2.779 (10)	151
Symmetry codes: (iv) $[x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (v) x, y, z+1; (vi) $[x+1, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (vii) $[x+1, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999 ); software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810035634/hy2346sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810035634/hy2346Isup2.hkl

checkCIF report

Comment top

In recent years, investigations on the design and synthesis of lanthanide-transition metal coordination polymers have attracted great interest not only for their fascinating structural topologies but also for their potential applications in magnetism, luminescence materials, molecular adsorption, and bimetallic catalysis (Cheng et al., 2007, 2008; Fan & Wu, 2010; Fang et al., 2009; Luo et al., 2007). Isonicotinic acid, which acts as a multidentate ligand possessing N and O donor atoms, is utilized to construct lanthanide-transition metal coordination polymers via the carboxylate group coordinating to lanthanide ions and N atom bonding to transition metal ions, such as Ag^I or Cu^I ions. We report herein the crystal structure of the title 4d-4f compound by the reaction of Gd₂O₃, isonicotinic acid and AgNO₃ under hydrothermal conditions.

As shown in Fig. 1, the asymmetric unit of the title compound contains one Gd^III ion, two Ag^I ions, four isonicotinate ligands, two coordinated water molecules, one nitrate ion, and one uncoordinated water molecule. The Gd^III ion is coordinated by eight O atoms from six isonicotinate ligands and two water molecules in a distorted square antiprismatic geometry, with the Gd—O bond lengths and O—Gd—O bond angles being from 2.356 (4) to 2.534 (4) Å and 71.22 (13) to 145.29 (14)°, respectively (Table 1). Each Ag^I ion is bonded to two N atoms from two different isonicotinate ligands in a linear or bow-like fashion, with the Ag—N bond lengths of 2.145 (5)–2.201 (5) Å and N—Ag—N bond angles of 178.5 (2)° and 147.30 (19) (Table 1). Adjacent Gd centers are connected by two carboxylate groups from two different isonicotinate ligands, forming one-dimensional chains, which are further linked by Ag^I ions to construct two-dimensional layers. The layers are stabilized by O—H···O hydrogen bonds involving the coordinated and uncoordinated water molecules (Table 2) and intralayer π–π stacking interactions between the pyridine rings, with centroid–centroid distances of 3.551 (4) and 3.555 (4) Å (Spek, 2009. The layers interact each other by interlayer Ag2···O10(aqua) contacts [2.731 (4) Å] and π–π stacking interactions between the pyridine rings from two neighboring layers, with centroid–centroid distances of 3.466 (3) and 3.516 (3) Å, which result in the formation of a three-dimensional supramolecular structure (Fig. 2).

Related literature top

For general background to the structures and properties of lanthanide–transition metal coordination polymers, see: Cheng et al. (2007, 2008); Fan & Wu (2010); Fang et al. (2009); Luo et al. (2007).

Experimental top

A mixture of Gd₂O₃ (0.181 g, 0.5 mmol), isonicotinic acid (0.123 g, 1 mmol), AgNO₃ (0.170 g, 1 mmol) and H₂O (10 ml) was placed in a 23 ml Teflon-lined reactor, which was heated to 443 K for 7 d and then cooled to room temperature at a rate of 0.2 K h^-1. The colorless crystals obtained were washed with water and dried in air (yield 32% based on Gd).

Computing details top

Data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear (Rigaku, 2007); data reduction: CrystalClear (Rigaku, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

Figures top

	Fig. 1. The asymmetric unit of the title compound. Displacement ellipsoids are drawn at the 30% probability level. Additional symmetry related atoms are included to complete the coordination geomtry around the Gd atom. [Symmetry code: (A) x, 1/2-y, 1/2+z.]
	Fig. 2. The three-dimensional supramolecular structure viewed along the c axis, formed through weak interlayer Ag···O contacts and π–π stacking interactions (dashed lines).

Poly[[diaquabis(µ₃-isonicotinato-κ³N:O:O')bis(µ₂- isonicotinato-κ²N:O)gadolinium(III)disiliver(I)] nitrate monohydrate] top

Crystal data top

[Ag₂Gd(C₆H₄NO₂)₄(H₂O)₂]NO₃·H₂O	F(000) = 1884
M_r = 977.46	D_x = 2.315 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 6663 reflections
a = 16.889 (8) Å	θ = 3.0–27.5°
b = 24.744 (11) Å	µ = 3.80 mm⁻¹
c = 6.750 (3) Å	T = 293 K
β = 96.240 (9)°	Block, colorless
V = 2804 (2) Å³	0.30 × 0.12 × 0.08 mm
Z = 4

Data collection top

Rigaku Mercury CCD diffractometer	4859 independent reflections
Radiation source: fine-focus sealed tube	4370 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.032
ω scans	θ_max = 25.0°, θ_min = 2.6°
Absorption correction: multi-scan (CrystalClear; Rigaku, 2007)	h = −20→19
T_min = 0.703, T_max = 1.000	k = −28→29
16445 measured reflections	l = −8→8

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.129	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.0925P)² + 0.0116P] where P = (F_o² + 2F_c²)/3
4859 reflections	(Δ/σ)_max = 0.002
416 parameters	Δρ_max = 1.38 e Å⁻³
0 restraints	Δρ_min = −1.27 e Å⁻³

Crystal data top

[Ag₂Gd(C₆H₄NO₂)₄(H₂O)₂]NO₃·H₂O	V = 2804 (2) Å³
M_r = 977.46	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 16.889 (8) Å	µ = 3.80 mm⁻¹
b = 24.744 (11) Å	T = 293 K
c = 6.750 (3) Å	0.30 × 0.12 × 0.08 mm
β = 96.240 (9)°

Data collection top

Rigaku Mercury CCD diffractometer	4859 independent reflections
Absorption correction: multi-scan (CrystalClear; Rigaku, 2007)	4370 reflections with I > 2σ(I)
T_min = 0.703, T_max = 1.000	R_int = 0.032
16445 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.034	0 restraints
wR(F²) = 0.129	H-atom parameters constrained
S = 1.08	Δρ_max = 1.38 e Å⁻³
4859 reflections	Δρ_min = −1.27 e Å⁻³
416 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Gd1	0.769985 (15)	0.162835 (10)	0.61682 (4)	0.01965 (14)
Ag1	1.27129 (3)	0.27098 (2)	0.49007 (9)	0.04268 (18)
Ag2	0.26502 (3)	0.00962 (2)	0.40147 (9)	0.04637 (19)
O1	0.8613 (2)	0.23037 (17)	0.5464 (8)	0.0399 (11)
O2	0.8530 (2)	0.31392 (15)	0.4284 (6)	0.0255 (8)
O3	0.8850 (2)	0.10782 (16)	0.6024 (6)	0.0309 (9)
O4	0.9135 (3)	0.05792 (18)	0.8754 (6)	0.0342 (10)
O5	0.6664 (3)	0.1044 (2)	0.4728 (6)	0.0412 (12)
O6	0.6514 (3)	0.08461 (19)	0.1515 (7)	0.0380 (11)
O7	0.6853 (2)	0.22994 (18)	0.4473 (7)	0.0394 (11)
O8	0.6733 (2)	0.31472 (17)	0.3362 (6)	0.0305 (9)
O9	0.7837 (3)	0.1483 (2)	0.2626 (6)	0.0419 (12)
H9A	0.7661	0.1161	0.2502	0.050*
H9B	0.8157	0.1639	0.1924	0.050*
O10	0.7581 (2)	0.08017 (15)	0.8329 (6)	0.0293 (9)
H10C	0.8059	0.0717	0.8722	0.035*
H10A	0.7353	0.0817	0.9390	0.035*
O11	0.2993 (4)	0.0486 (3)	0.8246 (9)	0.076 (2)
O12	0.2422 (4)	0.0839 (3)	1.0578 (9)	0.084 (2)
O13	0.2575 (5)	0.1295 (3)	0.7976 (11)	0.083 (2)
O14	1.2728 (4)	0.3429 (2)	0.9058 (12)	0.0660 (18)
H14C	1.2816	0.3432	1.0322	0.08 (4)*
H14B	1.2406	0.3619	0.8292	0.095*
N1	1.1448 (3)	0.2720 (2)	0.4982 (7)	0.0295 (11)
N2	1.1488 (3)	0.0291 (2)	0.4987 (8)	0.0319 (12)
N3	0.3875 (3)	0.0365 (2)	0.3745 (8)	0.0317 (11)
N4	0.3979 (3)	0.2720 (2)	0.4807 (8)	0.0326 (12)
N5	0.2680 (4)	0.0875 (3)	0.8983 (11)	0.0524 (17)
C1	1.1038 (3)	0.3187 (3)	0.4945 (9)	0.0300 (13)
H1A	1.1321	0.3510	0.4970	0.036*
C2	1.0215 (3)	0.3210 (2)	0.4872 (9)	0.0254 (12)
H2A	0.9952	0.3541	0.4804	0.030*
C3	0.9793 (3)	0.2732 (2)	0.4900 (8)	0.0192 (11)
C4	1.0219 (3)	0.2248 (2)	0.4990 (9)	0.0244 (12)
H4A	0.9951	0.1920	0.5020	0.029*
C5	1.1036 (4)	0.2255 (3)	0.5035 (9)	0.0306 (13)
H5A	1.1312	0.1929	0.5103	0.037*
C6	0.8906 (3)	0.2727 (2)	0.4838 (7)	0.0202 (11)
C7	1.0969 (4)	0.0607 (2)	0.3909 (10)	0.0319 (13)
H7A	1.1093	0.0724	0.2670	0.038*
C8	1.0253 (4)	0.0770 (2)	0.4541 (9)	0.0286 (13)
H8A	0.9897	0.0980	0.3723	0.034*
C9	1.0080 (3)	0.0614 (2)	0.6418 (8)	0.0209 (11)
C10	1.0615 (3)	0.0291 (2)	0.7561 (9)	0.0299 (13)
H10B	1.0514	0.0180	0.8826	0.036*
C11	1.1301 (4)	0.0136 (2)	0.6792 (10)	0.0325 (14)
H11A	1.1654	−0.0089	0.7558	0.039*
C12	0.9283 (3)	0.0766 (2)	0.7152 (8)	0.0229 (12)
C13	0.4339 (4)	0.0597 (3)	0.5286 (9)	0.0327 (14)
H13A	0.4127	0.0643	0.6490	0.039*
C14	0.5102 (4)	0.0765 (2)	0.5146 (10)	0.0326 (14)
H14A	0.5406	0.0910	0.6250	0.039*
C15	0.5418 (3)	0.0717 (2)	0.3342 (8)	0.0219 (11)
C16	0.4947 (4)	0.0496 (2)	0.1764 (8)	0.0294 (13)
H16A	0.5139	0.0462	0.0530	0.035*
C17	0.4192 (4)	0.0327 (3)	0.2018 (10)	0.0328 (14)
H17A	0.3883	0.0178	0.0930	0.039*
C18	0.6282 (3)	0.0883 (2)	0.3187 (8)	0.0231 (12)
C19	0.4396 (3)	0.2255 (2)	0.4717 (9)	0.0288 (13)
H19A	0.4125	0.1928	0.4741	0.035*
C20	0.5204 (3)	0.2245 (2)	0.4593 (8)	0.0234 (12)
H20A	0.5476	0.1918	0.4597	0.028*
C21	0.4397 (4)	0.3187 (3)	0.4771 (9)	0.0323 (14)
H21A	0.4130	0.3511	0.4912	0.039*
C22	0.5186 (3)	0.3206 (2)	0.4539 (9)	0.0260 (12)
H22A	0.5441	0.3536	0.4434	0.031*
C23	0.5604 (3)	0.2726 (2)	0.4462 (7)	0.0202 (11)
C24	0.6471 (3)	0.2728 (2)	0.4095 (8)	0.0232 (12)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Gd1	0.0133 (2)	0.0206 (2)	0.0256 (2)	−0.00073 (9)	0.00462 (13)	0.00042 (9)
Ag1	0.0119 (3)	0.0577 (4)	0.0593 (4)	−0.0001 (2)	0.0077 (2)	0.0006 (3)
Ag2	0.0197 (3)	0.0572 (4)	0.0642 (4)	0.0012 (2)	0.0137 (2)	0.0041 (3)
O1	0.016 (2)	0.032 (2)	0.071 (3)	−0.0077 (18)	0.004 (2)	0.019 (2)
O2	0.0152 (19)	0.028 (2)	0.033 (2)	0.0050 (17)	−0.0015 (16)	0.0059 (17)
O3	0.027 (2)	0.030 (2)	0.037 (2)	0.0107 (18)	0.0090 (19)	0.0024 (18)
O4	0.033 (2)	0.042 (3)	0.029 (2)	0.016 (2)	0.0073 (19)	0.0101 (19)
O5	0.036 (3)	0.056 (3)	0.030 (2)	−0.026 (2)	−0.002 (2)	−0.001 (2)
O6	0.029 (2)	0.054 (3)	0.033 (2)	−0.010 (2)	0.0116 (19)	−0.005 (2)
O7	0.016 (2)	0.041 (3)	0.061 (3)	0.0114 (19)	0.004 (2)	0.015 (2)
O8	0.019 (2)	0.035 (2)	0.039 (2)	−0.0045 (18)	0.0097 (18)	0.0090 (19)
O9	0.041 (3)	0.063 (3)	0.023 (2)	−0.022 (2)	0.0083 (19)	−0.002 (2)
O10	0.026 (2)	0.025 (2)	0.038 (2)	0.0025 (18)	0.0141 (18)	0.0036 (17)
O11	0.051 (4)	0.112 (6)	0.063 (4)	0.029 (4)	0.002 (3)	−0.033 (4)
O12	0.065 (4)	0.143 (7)	0.042 (3)	0.047 (4)	−0.002 (3)	−0.002 (3)
O13	0.102 (6)	0.068 (5)	0.081 (4)	−0.019 (4)	0.020 (4)	−0.007 (4)
O14	0.062 (4)	0.038 (3)	0.098 (6)	−0.002 (3)	0.007 (4)	−0.001 (3)
N1	0.015 (2)	0.042 (3)	0.032 (3)	−0.001 (2)	0.005 (2)	0.000 (2)
N2	0.018 (3)	0.034 (3)	0.045 (3)	−0.002 (2)	0.009 (2)	−0.006 (2)
N3	0.016 (2)	0.032 (3)	0.047 (3)	0.002 (2)	0.003 (2)	0.002 (2)
N4	0.018 (3)	0.036 (3)	0.045 (3)	0.001 (2)	0.012 (2)	−0.003 (2)
N5	0.030 (3)	0.063 (4)	0.064 (5)	0.002 (3)	0.006 (3)	−0.018 (4)
C1	0.016 (3)	0.030 (3)	0.044 (3)	−0.008 (3)	0.006 (3)	0.000 (3)
C2	0.015 (3)	0.023 (3)	0.039 (3)	−0.001 (2)	0.008 (2)	0.005 (2)
C3	0.014 (3)	0.022 (3)	0.022 (3)	−0.001 (2)	0.002 (2)	0.002 (2)
C4	0.016 (3)	0.023 (3)	0.034 (3)	0.000 (2)	0.003 (2)	0.001 (2)
C5	0.024 (3)	0.031 (3)	0.037 (3)	0.007 (3)	0.005 (3)	0.003 (3)
C6	0.016 (3)	0.027 (3)	0.018 (2)	−0.004 (2)	0.003 (2)	−0.004 (2)
C7	0.028 (3)	0.031 (3)	0.039 (3)	0.002 (3)	0.012 (3)	0.002 (3)
C8	0.023 (3)	0.024 (3)	0.040 (3)	0.004 (2)	0.006 (3)	−0.005 (2)
C9	0.020 (3)	0.021 (3)	0.022 (3)	0.001 (2)	−0.001 (2)	−0.001 (2)
C10	0.019 (3)	0.034 (3)	0.037 (3)	−0.003 (3)	0.007 (3)	0.003 (3)
C11	0.021 (3)	0.032 (3)	0.044 (4)	0.010 (3)	0.001 (3)	0.003 (3)
C12	0.022 (3)	0.022 (3)	0.025 (3)	0.004 (2)	0.006 (2)	−0.003 (2)
C13	0.034 (3)	0.034 (3)	0.032 (3)	−0.001 (3)	0.009 (3)	−0.006 (3)
C14	0.031 (3)	0.030 (3)	0.038 (3)	−0.008 (3)	0.009 (3)	−0.008 (3)
C15	0.020 (3)	0.013 (2)	0.033 (3)	−0.001 (2)	0.004 (2)	0.002 (2)
C16	0.031 (3)	0.033 (3)	0.023 (3)	−0.003 (3)	0.001 (2)	0.000 (2)
C17	0.022 (3)	0.036 (3)	0.039 (3)	−0.007 (3)	0.000 (3)	0.003 (3)
C18	0.024 (3)	0.021 (3)	0.024 (3)	−0.006 (2)	0.000 (2)	−0.002 (2)
C19	0.018 (3)	0.030 (3)	0.038 (3)	−0.004 (2)	0.002 (3)	0.003 (2)
C20	0.021 (3)	0.028 (3)	0.022 (3)	0.002 (2)	0.004 (2)	0.001 (2)
C21	0.023 (3)	0.028 (3)	0.048 (4)	0.004 (3)	0.015 (3)	−0.002 (3)
C22	0.021 (3)	0.024 (3)	0.032 (3)	−0.004 (2)	0.003 (2)	0.001 (2)
C23	0.017 (3)	0.029 (3)	0.015 (2)	−0.003 (2)	0.005 (2)	0.002 (2)
C24	0.018 (3)	0.028 (3)	0.025 (3)	−0.001 (2)	0.007 (2)	0.003 (2)

Geometric parameters (Å, º) top

Gd1—O1	2.357 (4)	N4—C19	1.354 (8)
Gd1—O2ⁱ	2.465 (4)	N4—Ag1ⁱⁱⁱ	2.147 (5)
Gd1—O3	2.383 (4)	C1—C2	1.388 (8)
Gd1—O5	2.393 (4)	C1—H1A	0.9300
Gd1—O7	2.399 (4)	C2—C3	1.383 (8)
Gd1—O8ⁱ	2.386 (4)	C2—H2A	0.9300
Gd1—O9	2.454 (4)	C3—C4	1.395 (7)
Gd1—O10	2.533 (4)	C3—C6	1.494 (7)
Ag1—N1	2.144 (5)	C4—C5	1.377 (8)
Ag1—N4ⁱⁱ	2.147 (5)	C4—H4A	0.9300
Ag2—N2ⁱⁱⁱ	2.189 (5)	C5—H5A	0.9300
Ag2—N3	2.199 (5)	C7—C8	1.385 (9)
O1—C6	1.252 (7)	C7—H7A	0.9300
O2—C6	1.238 (7)	C8—C9	1.386 (8)
O2—Gd1^iv	2.465 (4)	C8—H8A	0.9300
O3—C12	1.261 (7)	C9—C10	1.378 (8)
O4—C12	1.227 (7)	C9—C12	1.530 (8)
O5—C18	1.229 (7)	C10—C11	1.374 (8)
O6—C18	1.238 (7)	C10—H10B	0.9300
O7—C24	1.253 (7)	C11—H11A	0.9300
O8—C24	1.251 (7)	C13—C14	1.367 (9)
O8—Gd1^iv	2.386 (4)	C13—H13A	0.9300
O9—H9A	0.8500	C14—C15	1.387 (8)
O9—H9B	0.8500	C14—H14A	0.9300
O10—H10C	0.8500	C15—C16	1.371 (8)
O10—H10A	0.8500	C15—C18	1.531 (8)
O11—N5	1.229 (9)	C16—C17	1.370 (9)
O12—N5	1.208 (9)	C16—H16A	0.9300
O13—N5	1.244 (10)	C17—H17A	0.9300
O14—H14C	0.8500	C19—C20	1.377 (8)
O14—H14B	0.8500	C19—H19A	0.9300
N1—C1	1.345 (8)	C20—C23	1.377 (8)
N1—C5	1.348 (8)	C20—H20A	0.9300
N2—C7	1.331 (8)	C21—C22	1.359 (9)
N2—C11	1.348 (8)	C21—H21A	0.9300
N2—Ag2ⁱⁱ	2.189 (5)	C22—C23	1.384 (8)
N3—C17	1.338 (8)	C22—H22A	0.9300
N3—C13	1.359 (8)	C23—C24	1.512 (7)
N4—C21	1.354 (8)

O1—Gd1—O3	80.95 (15)	C2—C3—C6	121.5 (5)
O1—Gd1—O8ⁱ	117.84 (16)	C4—C3—C6	120.4 (5)
O3—Gd1—O8ⁱ	140.74 (14)	C5—C4—C3	120.1 (5)
O1—Gd1—O5	144.27 (17)	C5—C4—H4A	120.0
O3—Gd1—O5	101.65 (17)	C3—C4—H4A	120.0
O8ⁱ—Gd1—O5	82.71 (15)	N1—C5—C4	121.9 (6)
O1—Gd1—O7	77.42 (16)	N1—C5—H5A	119.1
O3—Gd1—O7	145.32 (15)	C4—C5—H5A	119.1
O8ⁱ—Gd1—O7	73.87 (15)	O2—C6—O1	125.6 (5)
O5—Gd1—O7	81.52 (18)	O2—C6—C3	118.8 (5)
O1—Gd1—O9	76.97 (17)	O1—C6—C3	115.4 (5)
O3—Gd1—O9	73.28 (16)	N2—C7—C8	123.3 (6)
O8ⁱ—Gd1—O9	141.49 (16)	N2—C7—H7A	118.4
O5—Gd1—O9	69.98 (15)	C8—C7—H7A	118.4
O7—Gd1—O9	75.62 (18)	C9—C8—C7	118.6 (6)
O1—Gd1—O2ⁱ	71.51 (16)	C9—C8—H8A	120.7
O3—Gd1—O2ⁱ	77.15 (14)	C7—C8—H8A	120.7
O8ⁱ—Gd1—O2ⁱ	77.31 (14)	C8—C9—C10	118.9 (5)
O5—Gd1—O2ⁱ	144.13 (14)	C8—C9—C12	120.6 (5)
O7—Gd1—O2ⁱ	119.97 (15)	C10—C9—C12	120.5 (5)
O9—Gd1—O2ⁱ	139.49 (14)	C11—C10—C9	118.6 (6)
O1—Gd1—O10	141.58 (15)	C11—C10—H10B	120.7
O3—Gd1—O10	71.24 (14)	C9—C10—H10B	120.7
O8ⁱ—Gd1—O10	74.21 (14)	N2—C11—C10	123.5 (6)
O5—Gd1—O10	69.25 (15)	N2—C11—H11A	118.2
O7—Gd1—O10	138.84 (14)	C10—C11—H11A	118.2
O9—Gd1—O10	117.66 (16)	O4—C12—O3	127.1 (5)
O2ⁱ—Gd1—O10	76.74 (14)	O4—C12—C9	117.6 (5)
N4ⁱⁱ—Ag1—N1	178.6 (2)	O3—C12—C9	115.3 (5)
N2ⁱⁱⁱ—Ag2—N3	147.1 (2)	N3—C13—C14	123.0 (6)
C6—O1—Gd1	162.4 (4)	N3—C13—H13A	118.5
C6—O2—Gd1^iv	132.5 (3)	C14—C13—H13A	118.5
C12—O3—Gd1	138.3 (4)	C13—C14—C15	119.3 (6)
C18—O5—Gd1	146.4 (4)	C13—C14—H14A	120.3
C24—O7—Gd1	161.8 (4)	C15—C14—H14A	120.3
C24—O8—Gd1^iv	137.2 (4)	C16—C15—C14	118.0 (5)
Gd1—O9—H9A	99.5	C16—C15—C18	122.1 (5)
Gd1—O9—H9B	127.5	C14—C15—C18	119.8 (5)
H9A—O9—H9B	127.5	C17—C16—C15	119.6 (5)
Gd1—O10—H10C	104.3	C17—C16—H16A	120.2
Gd1—O10—H10A	121.4	C15—C16—H16A	120.2
H10C—O10—H10A	104.5	N3—C17—C16	123.6 (6)
H14C—O14—H14B	129.5	N3—C17—H17A	118.2
C1—N1—C5	118.0 (5)	C16—C17—H17A	118.2
C1—N1—Ag1	121.4 (4)	O5—C18—O6	127.3 (6)
C5—N1—Ag1	120.6 (4)	O5—C18—C15	116.5 (5)
C7—N2—C11	117.1 (5)	O6—C18—C15	116.2 (5)
C7—N2—Ag2ⁱⁱ	121.6 (4)	N4—C19—C20	122.8 (5)
C11—N2—Ag2ⁱⁱ	121.0 (4)	N4—C19—H19A	118.6
C17—N3—C13	116.4 (5)	C20—C19—H19A	118.6
C17—N3—Ag2	121.3 (4)	C23—C20—C19	118.9 (5)
C13—N3—Ag2	122.2 (4)	C23—C20—H20A	120.5
C21—N4—C19	116.7 (5)	C19—C20—H20A	120.5
C21—N4—Ag1ⁱⁱⁱ	122.2 (4)	N4—C21—C22	123.4 (6)
C19—N4—Ag1ⁱⁱⁱ	121.0 (4)	N4—C21—H21A	118.3
O12—N5—O11	121.1 (9)	C22—C21—H21A	118.3
O12—N5—O13	120.3 (7)	C21—C22—C23	119.0 (5)
O11—N5—O13	118.4 (8)	C21—C22—H22A	120.5
N1—C1—C2	123.3 (6)	C23—C22—H22A	120.5
N1—C1—H1A	118.4	C20—C23—C22	118.9 (5)
C2—C1—H1A	118.4	C20—C23—C24	120.2 (5)
C3—C2—C1	118.6 (5)	C22—C23—C24	120.8 (5)
C3—C2—H2A	120.7	O7—C24—O8	125.9 (5)
C1—C2—H2A	120.7	O7—C24—C23	116.8 (5)
C2—C3—C4	118.1 (5)	O8—C24—C23	117.2 (5)

Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x+1, y, z; (iii) x−1, y, z; (iv) x, −y+1/2, z−1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O9—H9A···O6	0.85	2.13	2.771 (7)	132
O9—H9B···O2^iv	0.85	2.03	2.811 (6)	153
O10—H10A···O6^v	0.85	2.12	2.954 (6)	165
O10—H10C···O4	0.85	1.84	2.662 (6)	162
O14—H14B···O12^vi	0.85	2.27	2.960 (9)	139
O14—H14C···O13^vii	0.85	2.01	2.779 (10)	151

Symmetry codes: (iv) x, −y+1/2, z−1/2; (v) x, y, z+1; (vi) x+1, −y+1/2, z−1/2; (vii) x+1, −y+1/2, z+1/2.

Experimental details

Crystal data
Chemical formula	[Ag₂Gd(C₆H₄NO₂)₄(H₂O)₂]NO₃·H₂O
M_r	977.46
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	16.889 (8), 24.744 (11), 6.750 (3)
β (°)	96.240 (9)
V (Å³)	2804 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	3.80
Crystal size (mm)	0.30 × 0.12 × 0.08

Data collection
Diffractometer	Rigaku Mercury CCD diffractometer
Absorption correction	Multi-scan (CrystalClear; Rigaku, 2007)
T_min, T_max	0.703, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections	16445, 4859, 4370
R_int	0.032
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.034, 0.129, 1.08
No. of reflections	4859
No. of parameters	416
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.38, −1.27

Computer programs: CrystalClear (Rigaku, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999), SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

Selected bond lengths (Å) top

Gd1—O1	2.357 (4)	Gd1—O9	2.454 (4)
Gd1—O2ⁱ	2.465 (4)	Gd1—O10	2.533 (4)
Gd1—O3	2.383 (4)	Ag1—N1	2.144 (5)
Gd1—O5	2.393 (4)	Ag1—N4ⁱⁱ	2.147 (5)
Gd1—O7	2.399 (4)	Ag2—N2ⁱⁱⁱ	2.189 (5)
Gd1—O8ⁱ	2.386 (4)	Ag2—N3	2.199 (5)

Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x+1, y, z; (iii) x−1, y, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O9—H9A···O6	0.85	2.13	2.771 (7)	132
O9—H9B···O2^iv	0.85	2.03	2.811 (6)	153
O10—H10A···O6^v	0.85	2.12	2.954 (6)	165
O10—H10C···O4	0.85	1.84	2.662 (6)	162
O14—H14B···O12^vi	0.85	2.27	2.960 (9)	139
O14—H14C···O13^vii	0.85	2.01	2.779 (10)	151

Symmetry codes: (iv) x, −y+1/2, z−1/2; (v) x, y, z+1; (vi) x+1, −y+1/2, z−1/2; (vii) x+1, −y+1/2, z+1/2.

Acknowledgements

This work was supported financially by the Young Talent Fund of Fujian Province (No. 2007 F3060).

References

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