Literature DB >> 21583037

Poly[[aqua-bis(μ(3)-isonicotinato-κO:O':N)tris-(μ(2)-isonicotinato-κO,O':N)(nitrato-κO)bis-(μ(4)-oxalato-κO,O:O:O,O:O)dierbium(III)tetra-silver(I)] tetra-hydrate].

Yan-Mei Wen, Tian-Jun Feng, Li-Xin He.   

Abstract

In the title coordination polymer, {[Ag(4)Er(2)(C(6)H(4)NO(2))(5)(C(2)O(4))(2)(NO(3))(H(2)O)]·4H(2)O}(n), each Er(III) atom is coordinated in a bicapped trigonal-prismatic coordination geometry by three O atoms from two isonicotinate (IN) ligands, four O atoms from two n class="Chemical">oxalate ligands and one O atom from either a nitrate ion or a water mol-ecule, both of which are half-occupied over the same site. One Ag(I) 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 Ag(I) 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 Ag(I) ions. Due to the disorder, this IN ligand coordinates to the Ag atom through either the pyridyl N or the carboxyl-ate 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.

Entities:  

Year:  2009        PMID: 21583037      PMCID: PMC2969826          DOI: 10.1107/S160053680901842X

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


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

[Ag4Er2(C6H4NO2)5(C2O4)2(NO3)(H2O)]·4n class="Chemical">H2O M = 1704.64 Triclinic, a = 8.8561 (8) Å b = 11.6428 (8) Å c = 11.9597 (9) Å α = 76.940 (1)° β = 76.612 (1)° γ = 76.035 (1)° V = 1145.14 (16) Å3 Z = 1 Mo Kα radiation μ = 5.40 mm−1 T = 296 K 0.30 × 0.25 × 0.21 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.224, T max = 0.336 5823 measured reflections 4043 independent reflections 3265 reflections with I > 2σ(I) R int = 0.028

Refinement

R[F 2 > 2σ(F 2)] = 0.053 wR(F 2) = 0.128 S = 1.06 4043 reflections 377 parameters 95 restraints H-atom parameters constrained Δρmax = 1.57 e Å−3 Δρmin = −1.32 e Å−3 Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: 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 n class="Disease">DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680901842X/hy2195sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S160053680901842X/hy2195Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ag4Er2(C6H4NO2)5(C2O4)2(NO3)(H2O)]·4H2OZ = 1
Mr = 1704.64F(000) = 808
Triclinic, P1Dx = 2.472 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.8561 (8) ÅCell parameters from 2895 reflections
b = 11.6428 (8) Åθ = 2.4–27.9°
c = 11.9597 (9) ŵ = 5.40 mm1
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 diffractometer4043 independent reflections
Radiation source: fine-focus sealed tube3265 reflections with I > 2σ(I)
graphiteRint = 0.028
φ and ω scansθmax = 25.2°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −10→10
Tmin = 0.224, Tmax = 0.336k = −9→13
5823 measured reflectionsl = −12→14
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.053Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.128H-atom parameters constrained
S = 1.06w = 1/[σ2(Fo2) + (0.0536P)2 + 8.9026P] where P = (Fo2 + 2Fc2)/3
4043 reflections(Δ/σ)max = 0.001
377 parametersΔρmax = 1.57 e Å3
95 restraintsΔρmin = −1.32 e Å3
xyzUiso*/UeqOcc. (<1)
Er10.75631 (5)0.84475 (4)1.13533 (4)0.02560 (13)
Ag11.03061 (11)0.73575 (8)0.83111 (8)0.0482 (3)
Ag20.34657 (11)0.20986 (8)1.22733 (8)0.0471 (2)
C11.0226 (11)0.9620 (8)0.9516 (8)0.027 (2)
C20.4797 (11)1.0449 (8)1.0425 (8)0.027 (2)
C31.5447 (11)0.8125 (8)0.3439 (9)0.029 (2)
C41.4291 (12)0.7896 (9)0.4583 (9)0.034 (3)
C51.4180 (12)0.8533 (8)0.5437 (9)0.034 (3)
H51.48450.90700.53380.041*
C61.3046 (12)0.8368 (8)0.6469 (9)0.035 (3)
H61.29310.88340.70310.042*
C71.2262 (14)0.6927 (10)0.5844 (10)0.046 (3)
H71.16160.63700.59690.056*
C81.3334 (13)0.7052 (10)0.4786 (10)0.044 (3)
H81.34070.65850.42320.053*
C90.8121 (10)0.5945 (8)1.0183 (9)0.029 (2)
C100.7093 (11)0.5019 (8)1.0682 (9)0.030 (2)
C110.5937 (12)0.5111 (9)1.1686 (10)0.042 (3)
H110.58390.57351.20820.050*
C120.4945 (13)0.4316 (9)1.2108 (10)0.040 (3)
H120.41670.44211.27690.048*
C130.6205 (13)0.3255 (10)1.0633 (10)0.043 (3)
H130.62910.26131.02640.052*
C140.7232 (13)0.4003 (9)1.0175 (10)0.039 (3)
H140.80230.38510.95320.046*
N11.2105 (10)0.7535 (8)0.6665 (8)0.038 (2)
N20.5076 (10)0.3372 (7)1.1577 (7)0.032 (2)
O10.9558 (8)0.8752 (6)0.9658 (6)0.0322 (17)
O21.1251 (8)0.9947 (6)0.8621 (6)0.0335 (17)
O30.5567 (8)1.0219 (5)1.1240 (6)0.0308 (16)
O40.3750 (8)1.1387 (6)1.0208 (6)0.0323 (16)
O51.5301 (8)0.7718 (6)0.2569 (6)0.0358 (18)
O61.6484 (8)0.8716 (7)0.3354 (6)0.0425 (19)
O70.8188 (8)0.6624 (6)1.0829 (6)0.0359 (18)
O80.8790 (8)0.5966 (6)0.9143 (6)0.0387 (18)
O110.9834 (9)0.7560 (8)1.2154 (8)0.057 (2)
H11A1.02810.78091.25720.085*0.50
H11B0.99460.67761.24340.085*0.50
N30.995 (4)0.651 (2)1.281 (2)0.085 (8)0.50
O120.860 (3)0.612 (2)1.318 (2)0.088 (7)0.50
O131.125 (3)0.595 (3)1.313 (3)0.133 (12)0.50
O140.209 (2)0.3871 (14)0.4571 (16)0.063 (5)0.50
H14A0.12510.36510.45750.095*0.50
H14B0.18680.43040.50880.095*0.50
O151.035 (3)0.5205 (17)1.2890 (18)0.078 (6)0.50
H15A1.01730.49891.23150.117*0.50
H15B1.12340.48011.30180.117*0.50
O160.7488 (11)0.1435 (8)0.8439 (9)0.080 (3)
H16A0.82230.18140.82840.120*
H16B0.67980.18310.80450.120*
N50.1892 (14)0.1154 (11)1.3561 (10)0.037 (4)0.50
C150.1322 (18)0.0286 (12)1.3241 (10)0.042 (5)0.50
H150.16310.01351.24820.051*0.50
C160.029 (2)−0.0355 (13)1.4057 (13)0.049 (5)0.50
H16−0.0092−0.09351.38430.058*0.50
C17−0.0173 (19)−0.0129 (14)1.5192 (12)0.035 (4)0.50
C180.0398 (18)0.0739 (14)1.5512 (9)0.039 (4)0.50
H180.00880.08901.62710.047*0.50
C190.1430 (16)0.1380 (11)1.4696 (11)0.042 (5)0.50
H190.18120.19601.49100.050*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
U11U22U33U12U13U23
Er10.0229 (2)0.0283 (2)0.0268 (2)−0.01183 (17)0.00013 (17)−0.00509 (17)
Ag10.0470 (5)0.0600 (6)0.0354 (5)−0.0242 (4)0.0112 (4)−0.0090 (4)
Ag20.0507 (5)0.0476 (5)0.0445 (5)−0.0299 (4)0.0100 (4)−0.0089 (4)
C10.023 (5)0.032 (5)0.026 (5)−0.009 (4)0.002 (4)−0.005 (4)
C20.026 (5)0.027 (5)0.027 (5)−0.008 (4)0.001 (4)−0.004 (4)
C30.031 (5)0.021 (5)0.033 (6)−0.006 (4)−0.005 (4)−0.003 (4)
C40.029 (5)0.036 (6)0.032 (6)−0.004 (4)0.002 (4)−0.007 (5)
C50.043 (6)0.023 (5)0.035 (6)−0.019 (4)0.007 (5)−0.002 (4)
C60.046 (6)0.021 (5)0.038 (6)−0.010 (4)−0.006 (5)−0.004 (4)
C70.053 (7)0.046 (6)0.040 (7)−0.032 (5)0.014 (5)−0.010 (5)
C80.049 (6)0.042 (6)0.044 (7)−0.027 (5)0.015 (5)−0.019 (5)
C90.016 (4)0.026 (5)0.043 (6)−0.009 (4)−0.014 (4)0.012 (4)
C100.030 (5)0.028 (5)0.035 (6)−0.013 (4)−0.012 (4)0.003 (4)
C110.043 (6)0.031 (5)0.056 (7)−0.021 (5)0.013 (5)−0.027 (5)
C120.047 (6)0.037 (6)0.040 (6)−0.022 (5)0.005 (5)−0.015 (5)
C130.055 (7)0.035 (6)0.042 (7)−0.026 (5)0.002 (6)−0.007 (5)
C140.042 (6)0.035 (6)0.038 (6)−0.017 (5)0.006 (5)−0.010 (5)
N10.036 (5)0.043 (5)0.031 (5)−0.016 (4)0.009 (4)−0.004 (4)
N20.042 (5)0.021 (4)0.036 (5)−0.016 (4)−0.002 (4)−0.001 (3)
O10.034 (4)0.025 (3)0.036 (4)−0.018 (3)0.008 (3)−0.005 (3)
O20.037 (4)0.036 (4)0.034 (4)−0.023 (3)0.003 (3)−0.013 (3)
O30.033 (4)0.024 (3)0.039 (4)−0.002 (3)−0.011 (3)−0.012 (3)
O40.031 (4)0.037 (4)0.032 (4)−0.001 (3)−0.009 (3)−0.016 (3)
O50.036 (4)0.032 (4)0.039 (4)−0.017 (3)0.001 (3)−0.004 (3)
O60.039 (4)0.058 (5)0.036 (4)−0.034 (4)0.006 (3)−0.006 (3)
O70.038 (4)0.022 (3)0.049 (5)−0.014 (3)−0.005 (3)−0.004 (3)
O80.041 (4)0.035 (4)0.042 (5)−0.020 (3)−0.001 (4)−0.004 (3)
O110.052 (5)0.055 (5)0.068 (6)−0.011 (4)−0.033 (4)0.001 (4)
N30.12 (2)0.081 (17)0.087 (18)−0.060 (16)−0.025 (17)−0.036 (14)
O120.099 (15)0.086 (14)0.102 (17)−0.043 (13)−0.028 (13)−0.030 (12)
O130.099 (19)0.12 (2)0.14 (2)−0.004 (17)−0.052 (18)0.058 (18)
O140.054 (10)0.040 (9)0.082 (13)−0.013 (8)−0.005 (10)0.015 (9)
O150.121 (17)0.054 (11)0.080 (14)−0.036 (12)−0.042 (13)−0.010 (10)
O160.068 (6)0.064 (6)0.117 (9)−0.029 (5)−0.044 (6)0.010 (6)
N50.041 (10)0.028 (9)0.043 (8)−0.021 (7)0.005 (8)−0.003 (7)
C150.053 (12)0.037 (11)0.041 (10)−0.017 (9)−0.015 (8)0.000 (8)
C160.055 (12)0.039 (11)0.062 (9)−0.029 (9)−0.007 (9)−0.014 (8)
C170.020 (8)0.029 (9)0.057 (8)−0.009 (6)−0.009 (7)−0.003 (7)
C180.032 (10)0.043 (10)0.042 (9)−0.019 (7)0.003 (8)−0.007 (7)
C190.049 (12)0.029 (10)0.049 (10)−0.025 (8)0.002 (10)−0.007 (8)
C200.026 (10)0.029 (10)0.075 (10)−0.006 (7)−0.011 (9)0.018 (8)
O90.090 (13)0.125 (15)0.088 (14)−0.089 (12)0.001 (13)0.001 (11)
O100.053 (11)0.068 (13)0.072 (10)−0.016 (10)0.005 (10)0.011 (9)
Er1—O72.254 (7)C10—C111.392 (14)
Er1—O112.339 (8)C10—C141.415 (15)
Er1—O2i2.364 (7)C11—C121.365 (14)
Er1—O4ii2.369 (7)C11—H110.9300
Er1—O32.371 (6)C12—N21.357 (13)
Er1—O12.382 (6)C12—H120.9300
Er1—O5iii2.400 (6)C13—N21.332 (13)
Er1—O6iii2.423 (7)C13—C141.350 (14)
Ag1—N12.231 (8)C13—H130.9300
Ag1—O82.263 (7)C14—H140.9300
Ag1—O12.417 (7)O2—Er1i2.364 (7)
Ag2—N52.122 (9)O4—Er1ii2.369 (7)
Ag2—N22.199 (8)O5—Er1v2.400 (6)
Ag2—O9iv2.521 (9)O6—Er1v2.423 (7)
Ag2—O10iv2.492 (9)O11—N31.28 (3)
C1—O11.251 (11)O11—H11A0.8385
C1—O21.283 (11)O11—H11B0.8880
C1—C1i1.536 (19)N3—O131.28 (4)
C2—O31.260 (12)N3—O121.32 (3)
C2—O41.270 (11)O14—H14A0.8385
C2—C2ii1.545 (19)O14—H14B0.8436
C3—O61.248 (12)O15—H15A0.8402
C3—O51.280 (12)O15—H15B0.8410
C3—C41.519 (13)O16—H16A0.8365
C3—Er1v2.762 (10)O16—H16B0.8405
C4—C51.365 (15)N5—C151.3900
C4—C81.394 (14)N5—C191.3900
C5—C61.407 (14)C15—C161.3900
C5—H50.9300C15—H150.9300
C6—N11.374 (13)C16—C171.3900
C6—H60.9300C16—H160.9300
C7—N11.299 (14)C17—C181.3900
C7—C81.396 (15)C17—C201.57 (3)
C7—H70.9300C18—C191.3900
C8—H80.9300C18—H180.9300
C9—O71.243 (12)C19—H190.9300
C9—O81.246 (12)C20—O91.22 (3)
C9—C101.509 (13)C20—O101.24 (3)
O7—Er1—O1178.4 (3)C14—C10—C9123.0 (9)
O7—Er1—O2i140.7 (2)C12—C11—C10122.1 (10)
O11—Er1—O2i74.3 (3)C12—C11—H11118.9
O7—Er1—O4ii73.3 (2)C10—C11—H11118.9
O11—Er1—O4ii146.0 (3)N2—C12—C11121.0 (10)
O2i—Er1—O4ii118.2 (2)N2—C12—H12119.5
O7—Er1—O3139.7 (2)C11—C12—H12119.5
O11—Er1—O3141.7 (3)N2—C13—C14124.5 (10)
O2i—Er1—O373.1 (2)N2—C13—H13117.7
O4ii—Er1—O369.5 (2)C14—C13—H13117.7
O7—Er1—O178.8 (2)C13—C14—C10119.4 (10)
O11—Er1—O179.9 (3)C13—C14—H14120.3
O2i—Er1—O169.1 (2)C10—C14—H14120.3
O4ii—Er1—O176.4 (2)C7—N1—C6117.5 (9)
O3—Er1—O1106.1 (2)C7—N1—Ag1123.2 (7)
O7—Er1—O5iii83.7 (2)C6—N1—Ag1119.2 (7)
O11—Er1—O5iii110.4 (3)C13—N2—C12117.6 (9)
O2i—Er1—O5iii132.3 (2)C13—N2—Ag2122.1 (7)
O4ii—Er1—O5iii85.0 (2)C12—N2—Ag2120.4 (7)
O3—Er1—O5iii78.5 (2)C1—O1—Er1118.2 (6)
O1—Er1—O5iii157.4 (2)C1—O1—Ag1121.9 (6)
O7—Er1—O6iii122.2 (2)Er1—O1—Ag1119.9 (3)
O11—Er1—O6iii81.4 (3)C1—O2—Er1i118.2 (6)
O2i—Er1—O6iii81.1 (2)C2—O3—Er1117.8 (6)
O4ii—Er1—O6iii130.0 (2)C2—O4—Er1ii118.2 (6)
O3—Er1—O6iii74.3 (2)C3—O5—Er1v92.1 (6)
O1—Er1—O6iii148.1 (2)C3—O6—Er1v91.9 (6)
O5iii—Er1—O6iii54.4 (2)C9—O7—Er1150.9 (6)
N1—Ag1—O8132.0 (3)C9—O8—Ag1118.1 (6)
N1—Ag1—O1124.5 (3)N3—O11—Er1120.6 (14)
O8—Ag1—O1103.6 (2)N3—O11—H11A91.9
N5—Ag2—N2156.4 (4)Er1—O11—H11A130.9
O1—C1—O2125.7 (9)Er1—O11—H11B115.6
O1—C1—C1i117.7 (10)H11A—O11—H11B103.8
O2—C1—C1i116.6 (10)O13—N3—O11121 (3)
O3—C2—O4125.6 (9)O13—N3—O12123 (3)
O3—C2—C2ii117.8 (10)O11—N3—O12115 (3)
O4—C2—C2ii116.5 (11)O13—N3—H11B120.8
O6—C3—O5121.5 (9)O12—N3—H11B110.8
O6—C3—C4120.3 (9)N3—O13—H15B100.2
O5—C3—C4118.2 (9)H14A—O14—H14B106.6
O6—C3—Er1v61.3 (5)H15A—O15—H15B106.7
O5—C3—Er1v60.3 (5)H16A—O16—H16B107.4
C4—C3—Er1v177.8 (7)C15—N5—C19120.0
C5—C4—C8118.8 (9)C15—N5—Ag2118.0 (7)
C5—C4—C3119.4 (9)C19—N5—Ag2122.0 (7)
C8—C4—C3121.8 (10)N5—C15—C16120.0
C4—C5—C6119.2 (10)N5—C15—H15120.0
C4—C5—H5120.4C16—C15—H15120.0
C6—C5—H5120.4C15—C16—C17120.0
N1—C6—C5121.6 (10)C15—C16—H16120.0
N1—C6—H6119.2C17—C16—H16120.0
C5—C6—H6119.2C18—C17—C16120.0
N1—C7—C8124.5 (10)C18—C17—C20122.1 (15)
N1—C7—H7117.8C16—C17—C20117.9 (15)
C8—C7—H7117.8C17—C18—C19120.0
C4—C8—C7118.2 (10)C17—C18—H18120.0
C4—C8—H8120.9C19—C18—H18120.0
C7—C8—H8120.9C18—C19—N5120.0
O7—C9—O8126.5 (9)C18—C19—H19120.0
O7—C9—C10117.7 (9)N5—C19—H19120.0
O8—C9—C10115.7 (9)O9—C20—O10128 (2)
C11—C10—C14115.3 (9)O9—C20—C17118 (2)
C11—C10—C9121.7 (9)O10—C20—C17113 (2)
D—H···AD—HH···AD···AD—H···A
O14—H14A···O9vi0.842.392.81 (3)111
O14—H14B···O12vii0.841.992.62 (3)131
O16—H16A···O11viii0.841.952.773 (12)170
O16—H16B···O5ix0.842.062.862 (12)158
C6—H6···O20.932.533.371 (12)151
C11—H11···O5iii0.932.423.315 (8)162
C12—H12···O14x0.932.563.441 (2)158
Table 1

Selected bond lengths (Å)

Er1—O72.254 (7)
Er1—O112.339 (8)
Er1—O2i2.364 (7)
Er1—O4ii2.369 (7)
Er1—O32.371 (6)
Er1—O12.382 (6)
Er1—O5iii2.400 (6)
Er1—O6iii2.423 (7)
Ag1—N12.231 (8)
Ag1—O82.263 (7)
Ag1—O12.417 (7)
Ag2—N52.122 (9)
Ag2—N22.199 (8)
Ag2—O9iv2.521 (9)
Ag2—O10iv2.492 (9)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
O14—H14A⋯O9v0.842.392.81 (3)111
O14—H14B⋯O12vi0.841.992.62 (3)131
O16—H16A⋯O11vii0.841.952.773 (12)170
O16—H16B⋯O5viii0.842.062.862 (12)158
C6—H6⋯O20.932.533.371 (12)151
C11—H11⋯O5iii0.932.423.315 (8)162
C12—H12⋯O14ix0.932.563.441 (2)158

Symmetry codes: (iii) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) .

  7 in total

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Journal:  Chem Commun (Camb)       Date:  2006-01-20       Impact factor: 6.222

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Journal:  Chem Commun (Camb)       Date:  2006-02-20       Impact factor: 6.222

5.  A four-shell, nesting doll-like 3d-4f cluster containing 108 metal ions.

Authors:  Xiang-Jian Kong; Yan-Ping Ren; Wen-Xian Chen; La-Sheng Long; Zhiping Zheng; Rong-Bin Huang; Lan-Sun Zheng
Journal:  Angew Chem Int Ed Engl       Date:  2008       Impact factor: 15.336

6.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

7.  Metal carboxylates with open architectures.

Authors:  C N R Rao; Srinivasan Natarajan; R Vaidhyanathan
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  7 in total

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