catena-Poly[[diaqua­(isonicotinato-κ²O,O′)­dysprosium(III)]-di-μ-isonicotinato-κ⁴O:O′]

The title dysprosium coordination polymer [Dy(IN)₃(H₂O)₂]_n, where IN⁻ is the isonicotinate anion C₆H₄NO₂⁻, has been hydro­thermally synthesized. The polymer exhibits a doubly carboxyl­ate-bridged infinite chain-like structure with the metal center lying on a crystallographic twofold axis and coordinating by two carboxyl­ate O atoms from a chelating isonicotinate group (also lying on a twofold axis), four carboxyl­ate O atoms from four bridging isonicotinate ligands, and two water mol­ecules, to yield an eight-coordinate square-anti­prismatic geometry.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C)= 0.014 Å
• R factor = 0.041
• wR factor = 0.097
• Data-to-parameter ratio = 12.7

checkCIF/PLATON results

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Computing details

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1999); software used to prepare material for publication: SHELXTL.

catena-Poly[[diaqua(isonicotinato-κ²O,O')dysprosium(III)]- di-µ-isonicotinato-κ⁴O:O']

Crystal data

[Dy(C6H4NO2)3(H2O)2]	F(000) = 1100
Mr = 564.84	Dx = 1.784 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1847 reflections
a = 15.7886 (5) Å	θ = 2.6–25.1°
b = 14.1361 (3) Å	µ = 3.60 mm^−1
c = 9.5136 (2) Å	T = 295 K
β = 97.893 (4)°	Prism, colourless
V = 2103.22 (9) Å^3	0.42 × 0.20 × 0.12 mm
Z = 4

Data collection

Siemens SMART CCD diffractometer	1847 independent reflections
Radiation source: fine-focus sealed tube	1736 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.029
φ and ω scans	θmax = 25.1°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→18
Tmin = 0.43, Tmax = 0.65	k = −16→14
3097 measured reflections	l = −11→10

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.097	H atoms treated by a mixture of independent and constrained refinement
S = 1.14	w = 1/[σ^2(Fo^2) + 48.3362P] where P = (Fo^2 + 2Fc^2)/3
1847 reflections	(Δ/σ)max < 0.001
146 parameters	Δρmax = 0.78 e Å^−3
12 restraints	Δρmin = −0.80 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Dy	0.0000	−0.02014 (4)	0.2500	0.02526 (17)
O1	0.1311 (3)	−0.0577 (4)	0.3845 (5)	0.0370 (13)
O2	0.0909 (3)	−0.0269 (4)	0.5914 (5)	0.0385 (13)
O3	0.0498 (4)	0.1366 (4)	0.3430 (5)	0.0354 (12)
O4	0.0318 (4)	−0.1600 (4)	0.1269 (6)	0.0353 (13)
H1	0.059 (5)	−0.149 (6)	0.064 (9)	0.03 (2)*
H2	0.064 (7)	−0.195 (7)	0.167 (11)	0.06 (3)*
C1	0.1427 (4)	−0.0577 (5)	0.5167 (7)	0.0269 (15)
C2	0.2242 (5)	−0.1019 (5)	0.5895 (8)	0.0315 (16)
C3	0.2871 (5)	−0.1344 (6)	0.5139 (9)	0.041 (2)
H3A	0.2826	−0.1254	0.4164	0.049*
C4	0.3576 (6)	−0.1815 (7)	0.5879 (10)	0.049 (2)
H4A	0.3999	−0.2031	0.5367	0.059*
C5	0.3080 (7)	−0.1634 (8)	0.7964 (11)	0.067 (3)
H5A	0.3148	−0.1723	0.8942	0.080*
C6	0.2362 (6)	−0.1161 (8)	0.7347 (10)	0.059 (3)
H6A	0.1963	−0.0939	0.7900	0.071*
C7	0.0000	0.1810 (7)	0.2500	0.030 (2)
C8	0.0000	0.2852 (9)	0.2500	0.043 (3)
C9	0.0676 (9)	0.3342 (8)	0.3181 (14)	0.085 (4)
H9A	0.1134	0.3015	0.3677	0.102*
C10	0.0691 (11)	0.4320 (11)	0.3145 (17)	0.106 (5)
H10A	0.1175	0.4642	0.3561	0.128*
N1	0.3676 (5)	−0.1969 (6)	0.7259 (8)	0.053 (2)
N2	0.0000	0.4819 (14)	0.2500	0.151 (9)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Dy	0.0240 (3)	0.0305 (3)	0.0206 (2)	0.000	0.00098 (17)	0.000
O1	0.032 (3)	0.054 (4)	0.024 (3)	0.003 (3)	−0.001 (2)	0.000 (2)
O2	0.041 (3)	0.047 (3)	0.029 (3)	0.011 (3)	0.008 (2)	0.001 (2)
O3	0.044 (3)	0.034 (3)	0.026 (3)	−0.001 (3)	−0.002 (2)	−0.001 (2)
O4	0.045 (4)	0.037 (3)	0.025 (3)	0.010 (3)	0.008 (3)	0.005 (2)
C1	0.027 (4)	0.032 (4)	0.022 (4)	0.000 (3)	0.003 (3)	−0.001 (3)
C2	0.030 (4)	0.029 (4)	0.033 (4)	0.002 (3)	−0.003 (3)	−0.001 (3)
C3	0.034 (4)	0.053 (5)	0.035 (4)	0.005 (4)	0.004 (4)	−0.010 (4)
C4	0.039 (5)	0.052 (6)	0.055 (6)	0.012 (4)	0.000 (4)	−0.012 (4)
C5	0.063 (6)	0.092 (7)	0.044 (5)	0.024 (5)	0.001 (4)	0.004 (5)
C6	0.052 (6)	0.087 (8)	0.036 (5)	0.028 (5)	−0.003 (4)	0.006 (5)
C7	0.056 (7)	0.014 (5)	0.021 (5)	0.000	0.008 (5)	0.000
C8	0.061 (8)	0.037 (7)	0.031 (6)	0.000	0.004 (6)	0.000
C9	0.093 (9)	0.044 (7)	0.105 (10)	−0.010 (6)	−0.035 (8)	0.006 (6)
C10	0.108 (8)	0.075 (7)	0.125 (9)	−0.006 (7)	−0.023 (7)	0.003 (7)
N1	0.049 (5)	0.067 (6)	0.041 (4)	0.014 (4)	−0.004 (4)	−0.003 (4)
N2	0.15 (2)	0.066 (11)	0.22 (3)	0.000	−0.037 (18)	0.000

Geometric parameters (Å, º)

Dy—O2^i	2.318 (5)	C3—C4	1.401 (12)
Dy—O2^ii	2.318 (5)	C3—H3A	0.9300
Dy—O1^iii	2.340 (5)	C4—N1	1.319 (12)
Dy—O1	2.340 (5)	C4—H4A	0.9300
Dy—O4	2.387 (6)	C5—N1	1.318 (13)
Dy—O4^iii	2.387 (6)	C5—C6	1.375 (13)
Dy—O3	2.474 (5)	C5—H5A	0.9300
Dy—O3^iii	2.474 (5)	C6—H6A	0.9300
Dy—C7	2.843 (10)	C7—O3^iii	1.267 (7)
O1—C1	1.246 (8)	C7—C8	1.473 (15)
O2—C1	1.234 (8)	C8—C9	1.359 (13)
O2—Dy^i	2.318 (5)	C8—C9^iii	1.359 (13)
O3—C7	1.267 (7)	C9—C10	1.384 (17)
O4—H1	0.80 (9)	C9—H9A	0.9300
O4—H2	0.77 (11)	C10—N2	1.371 (17)
C1—C2	1.510 (10)	C10—H10A	0.9300
C2—C3	1.382 (11)	N2—C10^iii	1.371 (17)
C2—C6	1.383 (11)
O2^i—Dy—O2^ii	146.7 (3)	Dy—O4—H1	112 (6)
O2^i—Dy—O1^iii	80.83 (19)	Dy—O4—H2	117 (8)
O2^ii—Dy—O1^iii	106.82 (18)	H1—O4—H2	96 (9)
O2^i—Dy—O1	106.82 (18)	O2—C1—O1	124.3 (7)
O2^ii—Dy—O1	80.83 (19)	O2—C1—C2	118.2 (6)
O1^iii—Dy—O1	153.8 (3)	O1—C1—C2	117.5 (6)
O2^i—Dy—O4	138.4 (2)	C3—C2—C6	117.5 (8)
O2^ii—Dy—O4	74.2 (2)	C3—C2—C1	121.8 (7)
O1^iii—Dy—O4	76.9 (2)	C6—C2—C1	120.7 (7)
O1—Dy—O4	81.4 (2)	C2—C3—C4	118.4 (8)
O2^i—Dy—O4^iii	74.2 (2)	C2—C3—H3A	120.8
O2^ii—Dy—O4^iii	138.4 (2)	C4—C3—H3A	120.8
O1^iii—Dy—O4^iii	81.4 (2)	N1—C4—C3	123.8 (8)
O1—Dy—O4^iii	76.9 (2)	N1—C4—H4A	118.1
O4—Dy—O4^iii	68.1 (3)	C3—C4—H4A	118.1
O2^i—Dy—O3	72.87 (19)	N1—C5—C6	124.2 (10)
O2^ii—Dy—O3	77.36 (19)	N1—C5—H5A	117.9
O1^iii—Dy—O3	127.78 (19)	C6—C5—H5A	117.9
O1—Dy—O3	78.07 (19)	C5—C6—C2	119.3 (9)
O4—Dy—O3	147.1 (2)	C5—C6—H6A	120.3
O4^iii—Dy—O3	130.14 (19)	C2—C6—H6A	120.3
O2^i—Dy—O3^iii	77.36 (19)	O3^iii—C7—O3	120.6 (9)
O2^ii—Dy—O3^iii	72.87 (19)	O3^iii—C7—C8	119.7 (5)
O1^iii—Dy—O3^iii	78.07 (19)	O3—C7—C8	119.7 (5)
O1—Dy—O3^iii	127.78 (19)	O3^iii—C7—Dy	60.3 (5)
O4—Dy—O3^iii	130.14 (19)	O3—C7—Dy	60.3 (5)
O4^iii—Dy—O3^iii	147.1 (2)	C8—C7—Dy	180.000 (1)
O3—Dy—O3^iii	52.8 (2)	C9—C8—C9^iii	118.8 (14)
O2^i—Dy—C7	73.34 (15)	C9—C8—C7	120.6 (7)
O2^ii—Dy—C7	73.34 (15)	C9^iii—C8—C7	120.6 (7)
O1^iii—Dy—C7	103.10 (14)	C8—C9—C10	120.8 (12)
O1—Dy—C7	103.10 (14)	C8—C9—H9A	119.6
O4—Dy—C7	145.96 (15)	C10—C9—H9A	119.6
O4^iii—Dy—C7	145.96 (15)	N2—C10—C9	120.7 (15)
O3—Dy—C7	26.42 (12)	N2—C10—H10A	119.7
O3^iii—Dy—C7	26.42 (12)	C9—C10—H10A	119.7
C1—O1—Dy	123.3 (5)	C5—N1—C4	116.8 (8)
C1—O2—Dy^i	174.0 (5)	C10^iii—N2—C10	118 (2)
C7—O3—Dy	93.3 (5)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O4—H1···O3^ii	0.80 (9)	2.10 (9)	2.774 (8)	142 (7)
O4—H2···N1^iv	0.77 (11)	2.06 (11)	2.821 (10)	170 (11)

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