metal-organic compounds
Poly[[aquabis(μ3-isonicotinato-κ3O:O′:N)tris(μ2-isonicotinato-κ3O,O′:N)(nitrato-κO)bis(μ4-oxalato-κ6O1,O2:O2:O1′,O2′:O1′)dierbium(III)tetrasilver(I)] tetrahydrate]
aCollege of Science, Guangdong Ocean University, Zhanjiang 524088, People's Republic of China, bCollege of Mathematics, Physics and Software Engineering, Lanzhou Jiaotong University, Lanzhou 730070, People's Republic of China, and cSchool of Pharmacy, Guangdong Phamaceutical University, Guangzhou 510006, People's Republic of China
*Correspondence e-mail: wenym75@126.com
In the title coordination polymer, {[Ag4Er2(C6H4NO2)5(C2O4)2(NO3)(H2O)]·4H2O}n, each ErIII atom is coordinated in a bicapped trigonal–prismatic coordination geometry by three O atoms from two isonicotinate (IN) ligands, four O atoms from two oxalate ligands and one O atom from either a nitrate ion or a water molecule, both of which are half-occupied over the same site. One AgI atom has a Y-shaped geometry defined by one N atom from one IN ligand, one O atom from another IN ligand and one O atom from an oxalate ligand. The other AgI atom is coordinated by two IN ligands and one O atom from an oxalate ligand. One of the IN ligands is disordered over an inversion center and forms a bridge between two centrosymmetric AgI ions. Due to the disorder, this IN ligand coordinates to the Ag atom through either the pyridyl N or the carboxylate O atoms. The IN and oxalate ligands link the Er and Ag atoms into a three-dimensional coordination framework. O—H⋯O and C—H⋯O hydrogen bonds are observed in the crystal structure.
Related literature
For general background to coordination polymers and open framework materials, see: Barbour (2006); Kepert (2006); Kong et al. (2008); Rao et al. (2004); Zhang et al. (2005). For background to isonicotinate complexes, see: Gheorghe et al. (2002).
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2007); cell SAINT (Bruker, 2007); data reduction: SAINT; 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.
Supporting information
10.1107/S160053680901842X/hy2195sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S160053680901842X/hy2195Isup2.hkl
A mixture of Er2O3 (0.192 g, 0.5 mmol), AgNO3 (0.169 g, 1 mmol), isonicotinic acid (0.123 g, 1 mmol), oxalic acid (0.09 g, 1 mmol), HNO3 (0.12 ml) and H2O (10 ml) was placed in a 23 ml Teflon-lined reactor, which was heated to 433 K for 3 d and then cooled to room temperature at a rate of 10 K h-1. The pale-purple crystals obtained were washed with water and dried in air (yield 46% based on Er).
C-bound H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93 Å and with Uiso(H) = 1.2Ueq(C). Water H atoms were tentatively located in difference Fourier maps and were refined with distance restraints of O—H = 0.84 (1) and H···H = 1.35 (1) Å and with Uiso(H) = 1.5Ueq(O). The hightest peak is located 0.95 Å from Ag1 and the deepest hole is located 1.02 Å from Er1.
Data collection: APEX2 (Bruker, 2007); cell
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) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).Fig. 1. The asymmetric unit of the title compound, with the symmetry-related atoms to complete the Er coordination. Displacement ellipsoids are drawn at the 50% probability level. H atoms have been omitted for clarity. [Symmetry code: (i) 2 - x, 2 - y, 2 - z; (ii) 1 - x, 2 - y, 2 - z; (iii) -1 + x, y, 1 + z; (iv) -x, -y, 3 - z.] | |
Fig. 2. A packing view of the title compound. Hydrogen bonds are shown as dashed lines. |
[Ag4Er2(C6H4NO2)5(C2O4)2(NO3)(H2O)]·4H2O | Z = 1 |
Mr = 1704.64 | F(000) = 808 |
Triclinic, P1 | Dx = 2.472 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.8561 (8) Å | Cell parameters from 2895 reflections |
b = 11.6428 (8) Å | θ = 2.4–27.9° |
c = 11.9597 (9) Å | µ = 5.40 mm−1 |
α = 76.940 (1)° | T = 296 K |
β = 76.612 (1)° | Block, colorless |
γ = 76.035 (1)° | 0.30 × 0.25 × 0.21 mm |
V = 1145.14 (16) Å3 |
Bruker APEXII CCD diffractometer | 4043 independent reflections |
Radiation source: fine-focus sealed tube | 3265 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
ϕ and ω scans | θmax = 25.2°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→10 |
Tmin = 0.224, Tmax = 0.336 | k = −9→13 |
5823 measured reflections | l = −12→14 |
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)] = 0.053 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.128 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0536P)2 + 8.9026P] where P = (Fo2 + 2Fc2)/3 |
4043 reflections | (Δ/σ)max = 0.001 |
377 parameters | Δρmax = 1.57 e Å−3 |
95 restraints | Δρmin = −1.32 e Å−3 |
[Ag4Er2(C6H4NO2)5(C2O4)2(NO3)(H2O)]·4H2O | γ = 76.035 (1)° |
Mr = 1704.64 | V = 1145.14 (16) Å3 |
Triclinic, P1 | Z = 1 |
a = 8.8561 (8) Å | Mo Kα radiation |
b = 11.6428 (8) Å | µ = 5.40 mm−1 |
c = 11.9597 (9) Å | T = 296 K |
α = 76.940 (1)° | 0.30 × 0.25 × 0.21 mm |
β = 76.612 (1)° |
Bruker APEXII CCD diffractometer | 4043 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3265 reflections with I > 2σ(I) |
Tmin = 0.224, Tmax = 0.336 | Rint = 0.028 |
5823 measured reflections |
R[F2 > 2σ(F2)] = 0.053 | 95 restraints |
wR(F2) = 0.128 | H-atom parameters constrained |
S = 1.06 | Δρmax = 1.57 e Å−3 |
4043 reflections | Δρmin = −1.32 e Å−3 |
377 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Er1 | 0.75631 (5) | 0.84475 (4) | 1.13533 (4) | 0.02560 (13) | |
Ag1 | 1.03061 (11) | 0.73575 (8) | 0.83111 (8) | 0.0482 (3) | |
Ag2 | 0.34657 (11) | 0.20986 (8) | 1.22733 (8) | 0.0471 (2) | |
C1 | 1.0226 (11) | 0.9620 (8) | 0.9516 (8) | 0.027 (2) | |
C2 | 0.4797 (11) | 1.0449 (8) | 1.0425 (8) | 0.027 (2) | |
C3 | 1.5447 (11) | 0.8125 (8) | 0.3439 (9) | 0.029 (2) | |
C4 | 1.4291 (12) | 0.7896 (9) | 0.4583 (9) | 0.034 (3) | |
C5 | 1.4180 (12) | 0.8533 (8) | 0.5437 (9) | 0.034 (3) | |
H5 | 1.4845 | 0.9070 | 0.5338 | 0.041* | |
C6 | 1.3046 (12) | 0.8368 (8) | 0.6469 (9) | 0.035 (3) | |
H6 | 1.2931 | 0.8834 | 0.7031 | 0.042* | |
C7 | 1.2262 (14) | 0.6927 (10) | 0.5844 (10) | 0.046 (3) | |
H7 | 1.1616 | 0.6370 | 0.5969 | 0.056* | |
C8 | 1.3334 (13) | 0.7052 (10) | 0.4786 (10) | 0.044 (3) | |
H8 | 1.3407 | 0.6585 | 0.4232 | 0.053* | |
C9 | 0.8121 (10) | 0.5945 (8) | 1.0183 (9) | 0.029 (2) | |
C10 | 0.7093 (11) | 0.5019 (8) | 1.0682 (9) | 0.030 (2) | |
C11 | 0.5937 (12) | 0.5111 (9) | 1.1686 (10) | 0.042 (3) | |
H11 | 0.5839 | 0.5735 | 1.2082 | 0.050* | |
C12 | 0.4945 (13) | 0.4316 (9) | 1.2108 (10) | 0.040 (3) | |
H12 | 0.4167 | 0.4421 | 1.2769 | 0.048* | |
C13 | 0.6205 (13) | 0.3255 (10) | 1.0633 (10) | 0.043 (3) | |
H13 | 0.6291 | 0.2613 | 1.0264 | 0.052* | |
C14 | 0.7232 (13) | 0.4003 (9) | 1.0175 (10) | 0.039 (3) | |
H14 | 0.8023 | 0.3851 | 0.9532 | 0.046* | |
N1 | 1.2105 (10) | 0.7535 (8) | 0.6665 (8) | 0.038 (2) | |
N2 | 0.5076 (10) | 0.3372 (7) | 1.1577 (7) | 0.032 (2) | |
O1 | 0.9558 (8) | 0.8752 (6) | 0.9658 (6) | 0.0322 (17) | |
O2 | 1.1251 (8) | 0.9947 (6) | 0.8621 (6) | 0.0335 (17) | |
O3 | 0.5567 (8) | 1.0219 (5) | 1.1240 (6) | 0.0308 (16) | |
O4 | 0.3750 (8) | 1.1387 (6) | 1.0208 (6) | 0.0323 (16) | |
O5 | 1.5301 (8) | 0.7718 (6) | 0.2569 (6) | 0.0358 (18) | |
O6 | 1.6484 (8) | 0.8716 (7) | 0.3354 (6) | 0.0425 (19) | |
O7 | 0.8188 (8) | 0.6624 (6) | 1.0829 (6) | 0.0359 (18) | |
O8 | 0.8790 (8) | 0.5966 (6) | 0.9143 (6) | 0.0387 (18) | |
O11 | 0.9834 (9) | 0.7560 (8) | 1.2154 (8) | 0.057 (2) | |
H11A | 1.0281 | 0.7809 | 1.2572 | 0.085* | 0.50 |
H11B | 0.9946 | 0.6776 | 1.2434 | 0.085* | 0.50 |
N3 | 0.995 (4) | 0.651 (2) | 1.281 (2) | 0.085 (8) | 0.50 |
O12 | 0.860 (3) | 0.612 (2) | 1.318 (2) | 0.088 (7) | 0.50 |
O13 | 1.125 (3) | 0.595 (3) | 1.313 (3) | 0.133 (12) | 0.50 |
O14 | 0.209 (2) | 0.3871 (14) | 0.4571 (16) | 0.063 (5) | 0.50 |
H14A | 0.1251 | 0.3651 | 0.4575 | 0.095* | 0.50 |
H14B | 0.1868 | 0.4304 | 0.5088 | 0.095* | 0.50 |
O15 | 1.035 (3) | 0.5205 (17) | 1.2890 (18) | 0.078 (6) | 0.50 |
H15A | 1.0173 | 0.4989 | 1.2315 | 0.117* | 0.50 |
H15B | 1.1234 | 0.4801 | 1.3018 | 0.117* | 0.50 |
O16 | 0.7488 (11) | 0.1435 (8) | 0.8439 (9) | 0.080 (3) | |
H16A | 0.8223 | 0.1814 | 0.8284 | 0.120* | |
H16B | 0.6798 | 0.1831 | 0.8045 | 0.120* | |
N5 | 0.1892 (14) | 0.1154 (11) | 1.3561 (10) | 0.037 (4) | 0.50 |
C15 | 0.1322 (18) | 0.0286 (12) | 1.3241 (10) | 0.042 (5) | 0.50 |
H15 | 0.1631 | 0.0135 | 1.2482 | 0.051* | 0.50 |
C16 | 0.029 (2) | −0.0355 (13) | 1.4057 (13) | 0.049 (5) | 0.50 |
H16 | −0.0092 | −0.0935 | 1.3843 | 0.058* | 0.50 |
C17 | −0.0173 (19) | −0.0129 (14) | 1.5192 (12) | 0.035 (4) | 0.50 |
C18 | 0.0398 (18) | 0.0739 (14) | 1.5512 (9) | 0.039 (4) | 0.50 |
H18 | 0.0088 | 0.0890 | 1.6271 | 0.047* | 0.50 |
C19 | 0.1430 (16) | 0.1380 (11) | 1.4696 (11) | 0.042 (5) | 0.50 |
H19 | 0.1812 | 0.1960 | 1.4910 | 0.050* | 0.50 |
C20 | −0.136 (3) | −0.087 (2) | 1.607 (3) | 0.048 (5) | 0.50 |
O9 | −0.180 (3) | −0.162 (2) | 1.5730 (17) | 0.095 (7) | 0.50 |
O10 | −0.170 (2) | −0.0606 (18) | 1.7064 (16) | 0.070 (6) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Er1 | 0.0229 (2) | 0.0283 (2) | 0.0268 (2) | −0.01183 (17) | 0.00013 (17) | −0.00509 (17) |
Ag1 | 0.0470 (5) | 0.0600 (6) | 0.0354 (5) | −0.0242 (4) | 0.0112 (4) | −0.0090 (4) |
Ag2 | 0.0507 (5) | 0.0476 (5) | 0.0445 (5) | −0.0299 (4) | 0.0100 (4) | −0.0089 (4) |
C1 | 0.023 (5) | 0.032 (5) | 0.026 (5) | −0.009 (4) | 0.002 (4) | −0.005 (4) |
C2 | 0.026 (5) | 0.027 (5) | 0.027 (5) | −0.008 (4) | 0.001 (4) | −0.004 (4) |
C3 | 0.031 (5) | 0.021 (5) | 0.033 (6) | −0.006 (4) | −0.005 (4) | −0.003 (4) |
C4 | 0.029 (5) | 0.036 (6) | 0.032 (6) | −0.004 (4) | 0.002 (4) | −0.007 (5) |
C5 | 0.043 (6) | 0.023 (5) | 0.035 (6) | −0.019 (4) | 0.007 (5) | −0.002 (4) |
C6 | 0.046 (6) | 0.021 (5) | 0.038 (6) | −0.010 (4) | −0.006 (5) | −0.004 (4) |
C7 | 0.053 (7) | 0.046 (6) | 0.040 (7) | −0.032 (5) | 0.014 (5) | −0.010 (5) |
C8 | 0.049 (6) | 0.042 (6) | 0.044 (7) | −0.027 (5) | 0.015 (5) | −0.019 (5) |
C9 | 0.016 (4) | 0.026 (5) | 0.043 (6) | −0.009 (4) | −0.014 (4) | 0.012 (4) |
C10 | 0.030 (5) | 0.028 (5) | 0.035 (6) | −0.013 (4) | −0.012 (4) | 0.003 (4) |
C11 | 0.043 (6) | 0.031 (5) | 0.056 (7) | −0.021 (5) | 0.013 (5) | −0.027 (5) |
C12 | 0.047 (6) | 0.037 (6) | 0.040 (6) | −0.022 (5) | 0.005 (5) | −0.015 (5) |
C13 | 0.055 (7) | 0.035 (6) | 0.042 (7) | −0.026 (5) | 0.002 (6) | −0.007 (5) |
C14 | 0.042 (6) | 0.035 (6) | 0.038 (6) | −0.017 (5) | 0.006 (5) | −0.010 (5) |
N1 | 0.036 (5) | 0.043 (5) | 0.031 (5) | −0.016 (4) | 0.009 (4) | −0.004 (4) |
N2 | 0.042 (5) | 0.021 (4) | 0.036 (5) | −0.016 (4) | −0.002 (4) | −0.001 (3) |
O1 | 0.034 (4) | 0.025 (3) | 0.036 (4) | −0.018 (3) | 0.008 (3) | −0.005 (3) |
O2 | 0.037 (4) | 0.036 (4) | 0.034 (4) | −0.023 (3) | 0.003 (3) | −0.013 (3) |
O3 | 0.033 (4) | 0.024 (3) | 0.039 (4) | −0.002 (3) | −0.011 (3) | −0.012 (3) |
O4 | 0.031 (4) | 0.037 (4) | 0.032 (4) | −0.001 (3) | −0.009 (3) | −0.016 (3) |
O5 | 0.036 (4) | 0.032 (4) | 0.039 (4) | −0.017 (3) | 0.001 (3) | −0.004 (3) |
O6 | 0.039 (4) | 0.058 (5) | 0.036 (4) | −0.034 (4) | 0.006 (3) | −0.006 (3) |
O7 | 0.038 (4) | 0.022 (3) | 0.049 (5) | −0.014 (3) | −0.005 (3) | −0.004 (3) |
O8 | 0.041 (4) | 0.035 (4) | 0.042 (5) | −0.020 (3) | −0.001 (4) | −0.004 (3) |
O11 | 0.052 (5) | 0.055 (5) | 0.068 (6) | −0.011 (4) | −0.033 (4) | 0.001 (4) |
N3 | 0.12 (2) | 0.081 (17) | 0.087 (18) | −0.060 (16) | −0.025 (17) | −0.036 (14) |
O12 | 0.099 (15) | 0.086 (14) | 0.102 (17) | −0.043 (13) | −0.028 (13) | −0.030 (12) |
O13 | 0.099 (19) | 0.12 (2) | 0.14 (2) | −0.004 (17) | −0.052 (18) | 0.058 (18) |
O14 | 0.054 (10) | 0.040 (9) | 0.082 (13) | −0.013 (8) | −0.005 (10) | 0.015 (9) |
O15 | 0.121 (17) | 0.054 (11) | 0.080 (14) | −0.036 (12) | −0.042 (13) | −0.010 (10) |
O16 | 0.068 (6) | 0.064 (6) | 0.117 (9) | −0.029 (5) | −0.044 (6) | 0.010 (6) |
N5 | 0.041 (10) | 0.028 (9) | 0.043 (8) | −0.021 (7) | 0.005 (8) | −0.003 (7) |
C15 | 0.053 (12) | 0.037 (11) | 0.041 (10) | −0.017 (9) | −0.015 (8) | 0.000 (8) |
C16 | 0.055 (12) | 0.039 (11) | 0.062 (9) | −0.029 (9) | −0.007 (9) | −0.014 (8) |
C17 | 0.020 (8) | 0.029 (9) | 0.057 (8) | −0.009 (6) | −0.009 (7) | −0.003 (7) |
C18 | 0.032 (10) | 0.043 (10) | 0.042 (9) | −0.019 (7) | 0.003 (8) | −0.007 (7) |
C19 | 0.049 (12) | 0.029 (10) | 0.049 (10) | −0.025 (8) | 0.002 (10) | −0.007 (8) |
C20 | 0.026 (10) | 0.029 (10) | 0.075 (10) | −0.006 (7) | −0.011 (9) | 0.018 (8) |
O9 | 0.090 (13) | 0.125 (15) | 0.088 (14) | −0.089 (12) | 0.001 (13) | 0.001 (11) |
O10 | 0.053 (11) | 0.068 (13) | 0.072 (10) | −0.016 (10) | 0.005 (10) | 0.011 (9) |
Er1—O7 | 2.254 (7) | C10—C11 | 1.392 (14) |
Er1—O11 | 2.339 (8) | C10—C14 | 1.415 (15) |
Er1—O2i | 2.364 (7) | C11—C12 | 1.365 (14) |
Er1—O4ii | 2.369 (7) | C11—H11 | 0.9300 |
Er1—O3 | 2.371 (6) | C12—N2 | 1.357 (13) |
Er1—O1 | 2.382 (6) | C12—H12 | 0.9300 |
Er1—O5iii | 2.400 (6) | C13—N2 | 1.332 (13) |
Er1—O6iii | 2.423 (7) | C13—C14 | 1.350 (14) |
Ag1—N1 | 2.231 (8) | C13—H13 | 0.9300 |
Ag1—O8 | 2.263 (7) | C14—H14 | 0.9300 |
Ag1—O1 | 2.417 (7) | O2—Er1i | 2.364 (7) |
Ag2—N5 | 2.122 (9) | O4—Er1ii | 2.369 (7) |
Ag2—N2 | 2.199 (8) | O5—Er1v | 2.400 (6) |
Ag2—O9iv | 2.521 (9) | O6—Er1v | 2.423 (7) |
Ag2—O10iv | 2.492 (9) | O11—N3 | 1.28 (3) |
C1—O1 | 1.251 (11) | O11—H11A | 0.8385 |
C1—O2 | 1.283 (11) | O11—H11B | 0.8880 |
C1—C1i | 1.536 (19) | N3—O13 | 1.28 (4) |
C2—O3 | 1.260 (12) | N3—O12 | 1.32 (3) |
C2—O4 | 1.270 (11) | O14—H14A | 0.8385 |
C2—C2ii | 1.545 (19) | O14—H14B | 0.8436 |
C3—O6 | 1.248 (12) | O15—H15A | 0.8402 |
C3—O5 | 1.280 (12) | O15—H15B | 0.8410 |
C3—C4 | 1.519 (13) | O16—H16A | 0.8365 |
C3—Er1v | 2.762 (10) | O16—H16B | 0.8405 |
C4—C5 | 1.365 (15) | N5—C15 | 1.3900 |
C4—C8 | 1.394 (14) | N5—C19 | 1.3900 |
C5—C6 | 1.407 (14) | C15—C16 | 1.3900 |
C5—H5 | 0.9300 | C15—H15 | 0.9300 |
C6—N1 | 1.374 (13) | C16—C17 | 1.3900 |
C6—H6 | 0.9300 | C16—H16 | 0.9300 |
C7—N1 | 1.299 (14) | C17—C18 | 1.3900 |
C7—C8 | 1.396 (15) | C17—C20 | 1.57 (3) |
C7—H7 | 0.9300 | C18—C19 | 1.3900 |
C8—H8 | 0.9300 | C18—H18 | 0.9300 |
C9—O7 | 1.243 (12) | C19—H19 | 0.9300 |
C9—O8 | 1.246 (12) | C20—O9 | 1.22 (3) |
C9—C10 | 1.509 (13) | C20—O10 | 1.24 (3) |
O7—Er1—O11 | 78.4 (3) | C14—C10—C9 | 123.0 (9) |
O7—Er1—O2i | 140.7 (2) | C12—C11—C10 | 122.1 (10) |
O11—Er1—O2i | 74.3 (3) | C12—C11—H11 | 118.9 |
O7—Er1—O4ii | 73.3 (2) | C10—C11—H11 | 118.9 |
O11—Er1—O4ii | 146.0 (3) | N2—C12—C11 | 121.0 (10) |
O2i—Er1—O4ii | 118.2 (2) | N2—C12—H12 | 119.5 |
O7—Er1—O3 | 139.7 (2) | C11—C12—H12 | 119.5 |
O11—Er1—O3 | 141.7 (3) | N2—C13—C14 | 124.5 (10) |
O2i—Er1—O3 | 73.1 (2) | N2—C13—H13 | 117.7 |
O4ii—Er1—O3 | 69.5 (2) | C14—C13—H13 | 117.7 |
O7—Er1—O1 | 78.8 (2) | C13—C14—C10 | 119.4 (10) |
O11—Er1—O1 | 79.9 (3) | C13—C14—H14 | 120.3 |
O2i—Er1—O1 | 69.1 (2) | C10—C14—H14 | 120.3 |
O4ii—Er1—O1 | 76.4 (2) | C7—N1—C6 | 117.5 (9) |
O3—Er1—O1 | 106.1 (2) | C7—N1—Ag1 | 123.2 (7) |
O7—Er1—O5iii | 83.7 (2) | C6—N1—Ag1 | 119.2 (7) |
O11—Er1—O5iii | 110.4 (3) | C13—N2—C12 | 117.6 (9) |
O2i—Er1—O5iii | 132.3 (2) | C13—N2—Ag2 | 122.1 (7) |
O4ii—Er1—O5iii | 85.0 (2) | C12—N2—Ag2 | 120.4 (7) |
O3—Er1—O5iii | 78.5 (2) | C1—O1—Er1 | 118.2 (6) |
O1—Er1—O5iii | 157.4 (2) | C1—O1—Ag1 | 121.9 (6) |
O7—Er1—O6iii | 122.2 (2) | Er1—O1—Ag1 | 119.9 (3) |
O11—Er1—O6iii | 81.4 (3) | C1—O2—Er1i | 118.2 (6) |
O2i—Er1—O6iii | 81.1 (2) | C2—O3—Er1 | 117.8 (6) |
O4ii—Er1—O6iii | 130.0 (2) | C2—O4—Er1ii | 118.2 (6) |
O3—Er1—O6iii | 74.3 (2) | C3—O5—Er1v | 92.1 (6) |
O1—Er1—O6iii | 148.1 (2) | C3—O6—Er1v | 91.9 (6) |
O5iii—Er1—O6iii | 54.4 (2) | C9—O7—Er1 | 150.9 (6) |
N1—Ag1—O8 | 132.0 (3) | C9—O8—Ag1 | 118.1 (6) |
N1—Ag1—O1 | 124.5 (3) | N3—O11—Er1 | 120.6 (14) |
O8—Ag1—O1 | 103.6 (2) | N3—O11—H11A | 91.9 |
N5—Ag2—N2 | 156.4 (4) | Er1—O11—H11A | 130.9 |
O1—C1—O2 | 125.7 (9) | Er1—O11—H11B | 115.6 |
O1—C1—C1i | 117.7 (10) | H11A—O11—H11B | 103.8 |
O2—C1—C1i | 116.6 (10) | O13—N3—O11 | 121 (3) |
O3—C2—O4 | 125.6 (9) | O13—N3—O12 | 123 (3) |
O3—C2—C2ii | 117.8 (10) | O11—N3—O12 | 115 (3) |
O4—C2—C2ii | 116.5 (11) | O13—N3—H11B | 120.8 |
O6—C3—O5 | 121.5 (9) | O12—N3—H11B | 110.8 |
O6—C3—C4 | 120.3 (9) | N3—O13—H15B | 100.2 |
O5—C3—C4 | 118.2 (9) | H14A—O14—H14B | 106.6 |
O6—C3—Er1v | 61.3 (5) | H15A—O15—H15B | 106.7 |
O5—C3—Er1v | 60.3 (5) | H16A—O16—H16B | 107.4 |
C4—C3—Er1v | 177.8 (7) | C15—N5—C19 | 120.0 |
C5—C4—C8 | 118.8 (9) | C15—N5—Ag2 | 118.0 (7) |
C5—C4—C3 | 119.4 (9) | C19—N5—Ag2 | 122.0 (7) |
C8—C4—C3 | 121.8 (10) | N5—C15—C16 | 120.0 |
C4—C5—C6 | 119.2 (10) | N5—C15—H15 | 120.0 |
C4—C5—H5 | 120.4 | C16—C15—H15 | 120.0 |
C6—C5—H5 | 120.4 | C15—C16—C17 | 120.0 |
N1—C6—C5 | 121.6 (10) | C15—C16—H16 | 120.0 |
N1—C6—H6 | 119.2 | C17—C16—H16 | 120.0 |
C5—C6—H6 | 119.2 | C18—C17—C16 | 120.0 |
N1—C7—C8 | 124.5 (10) | C18—C17—C20 | 122.1 (15) |
N1—C7—H7 | 117.8 | C16—C17—C20 | 117.9 (15) |
C8—C7—H7 | 117.8 | C17—C18—C19 | 120.0 |
C4—C8—C7 | 118.2 (10) | C17—C18—H18 | 120.0 |
C4—C8—H8 | 120.9 | C19—C18—H18 | 120.0 |
C7—C8—H8 | 120.9 | C18—C19—N5 | 120.0 |
O7—C9—O8 | 126.5 (9) | C18—C19—H19 | 120.0 |
O7—C9—C10 | 117.7 (9) | N5—C19—H19 | 120.0 |
O8—C9—C10 | 115.7 (9) | O9—C20—O10 | 128 (2) |
C11—C10—C14 | 115.3 (9) | O9—C20—C17 | 118 (2) |
C11—C10—C9 | 121.7 (9) | O10—C20—C17 | 113 (2) |
Symmetry codes: (i) −x+2, −y+2, −z+2; (ii) −x+1, −y+2, −z+2; (iii) x−1, y, z+1; (iv) −x, −y, −z+3; (v) x+1, y, z−1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O14—H14A···O9vi | 0.84 | 2.39 | 2.81 (3) | 111 |
O14—H14B···O12vii | 0.84 | 1.99 | 2.62 (3) | 131 |
O16—H16A···O11viii | 0.84 | 1.95 | 2.773 (12) | 170 |
O16—H16B···O5ix | 0.84 | 2.06 | 2.862 (12) | 158 |
C6—H6···O2 | 0.93 | 2.53 | 3.371 (12) | 151 |
C11—H11···O5iii | 0.93 | 2.42 | 3.315 (8) | 162 |
C12—H12···O14x | 0.93 | 2.56 | 3.441 (2) | 158 |
Symmetry codes: (iii) x−1, y, z+1; (vi) −x, −y, −z+2; (vii) −x+1, −y+1, −z+2; (viii) −x+2, −y+1, −z+2; (ix) −x+2, −y+1, −z+1; (x) x, y, z+1. |
Experimental details
Crystal data | |
Chemical formula | [Ag4Er2(C6H4NO2)5(C2O4)2(NO3)(H2O)]·4H2O |
Mr | 1704.64 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 296 |
a, b, c (Å) | 8.8561 (8), 11.6428 (8), 11.9597 (9) |
α, β, γ (°) | 76.940 (1), 76.612 (1), 76.035 (1) |
V (Å3) | 1145.14 (16) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 5.40 |
Crystal size (mm) | 0.30 × 0.25 × 0.21 |
Data collection | |
Diffractometer | Bruker APEXII CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.224, 0.336 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5823, 4043, 3265 |
Rint | 0.028 |
(sin θ/λ)max (Å−1) | 0.599 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.053, 0.128, 1.06 |
No. of reflections | 4043 |
No. of parameters | 377 |
No. of restraints | 95 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.57, −1.32 |
Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999), SHELXTL (Sheldrick, 2008).
Er1—O7 | 2.254 (7) | Ag1—N1 | 2.231 (8) |
Er1—O11 | 2.339 (8) | Ag1—O8 | 2.263 (7) |
Er1—O2i | 2.364 (7) | Ag1—O1 | 2.417 (7) |
Er1—O4ii | 2.369 (7) | Ag2—N5 | 2.122 (9) |
Er1—O3 | 2.371 (6) | Ag2—N2 | 2.199 (8) |
Er1—O1 | 2.382 (6) | Ag2—O9iv | 2.521 (9) |
Er1—O5iii | 2.400 (6) | Ag2—O10iv | 2.492 (9) |
Er1—O6iii | 2.423 (7) |
Symmetry codes: (i) −x+2, −y+2, −z+2; (ii) −x+1, −y+2, −z+2; (iii) x−1, y, z+1; (iv) −x, −y, −z+3. |
D—H···A | D—H | H···A | D···A | D—H···A |
O14—H14A···O9v | 0.84 | 2.39 | 2.81 (3) | 111 |
O14—H14B···O12vi | 0.84 | 1.99 | 2.62 (3) | 131 |
O16—H16A···O11vii | 0.84 | 1.95 | 2.773 (12) | 170 |
O16—H16B···O5viii | 0.84 | 2.06 | 2.862 (12) | 158 |
C6—H6···O2 | 0.93 | 2.53 | 3.371 (12) | 151 |
C11—H11···O5iii | 0.93 | 2.42 | 3.315 (8) | 162 |
C12—H12···O14ix | 0.93 | 2.56 | 3.441 (2) | 158 |
Symmetry codes: (iii) x−1, y, z+1; (v) −x, −y, −z+2; (vi) −x+1, −y+1, −z+2; (vii) −x+2, −y+1, −z+2; (viii) −x+2, −y+1, −z+1; (ix) x, y, z+1. |
Acknowledgements
The authors kindly acknowledge Guangdong Ocean University for supporting this work.
References
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This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
The design and construction of transition-lanthanide metal complexes have gained great recognition over the last decade because of their intriguing network topologies and potential applications, and due to their magnetic properties, their capacity for gas storage, as luminescent materials, and so on (Barbour, 2006; Kepert, 2006; Kong et al., 2008; Rao et al., 2004; Zhang et al., 2005). Isonicotinic acid is a multifunctional bridging ligand possessing of oxygen and nitrogen donors, which can thus be utilized to construct lanthanide-transition heterometallic complexes via the carboxyl oxygen atoms binding to lanthanides and nitrogen atoms bonding to transition metal ions such as AgI or CuI ions (Gheorghe et al., 2002). On the basis of above considerations, we chose nicotinic acid, mixed 4 d–4f metal ions and nitric acid as our building blocks. A new three-dimensional 4 d–4f coordination framework resulted from the hydrothermal treatment of Er2O3, AgNO3, oxalic acid, isonicotinic acid and nitric acid in water.
As depicted in Fig. 1, the asymmetric unit of the title compound contains one ErIII atom, two AgI atoms, two and a half IN ligands, two half oxalate anions, each on an inversion center, a half-occupied nitrate ion, a half-occupied coordinated water molecule and two uncoordinated water molecules. The ErIII atom is eight-coordinated in a bicapped trigonal prism coordination geometry by three O atoms from two IN ligands, four O atoms from two oxalate ligands and one O atom from either a nitrate ion or a water molecule, both of which are half-occupied over the same site (Table 1). The Ag1 atom is located in a Y-shaped configuration, defined by one N atom from one IN ligand, one O atom from another IN ligand and one O atom from one oxalate ligand. One of the IN ligands is disordered on an inversion center halfway between two Ag2 atoms and forms a bridge between the two Ag2 atoms. Due to the inversion disorder of this IN ligand, Ag2 is thus coordinated either to two N atoms or to a pyridyl N and two carboxylate O atoms from two IN ligands. In the crystal structure, a zigzag Er–oxalate–Ag chain is formed via the oxalate ligand. The chains are linked by pillared IN ligands to form a two-dimensional layer. The layers are further interconnected by Ag2(IN)3 units to form a three-dimensional coordination framework. The supramolecular structure are further stabilized by O—H···O and C—H···O hydrogen bonds involving the carboxylate groups, uncoordinated water molecules and disordered nitrate ions (Table 2; Fig. 2).