Poly[[triaqua-(μ(3)-4-oxidopyridine-2,6-dicarboxyl-ato)holmium(III)] mono-hydrate].

In the title coordination polymer, {[Ho(C(7)H(2)NO(5))(H(2)O)(3)]·H(2)O}(n), the Ho(III) atom is eight-coordinated by a tridentate 4-oxidopyridine-2,6-dicarboxyl-ate trianion, two monodentate anions and three water mol-ecules, forming a distorted bicapped trigonal-prismatic HoNO(7) coordination geometry. The anions bridge adjacent Ho(III) ions into double chains. Adjacent chains are further connected into sheets. O-H⋯O hydrogen bonds involving both coordinated and uncoordinated water mol-ecules generate a three-dimensional supra-molecular framework.

Related literature

For the structures and properties of lanthanide coordination compounds, see: Wang et al. (2007 ▶); Lv et al. (2010 ▶); Gao et al. (2006 ▶). For bond lengths and angles in other complexes with eight-coordinate n class="Chemical">HoIII, see: Wang et al. (2007 ▶); Munoz et al. (2005 ▶).

Experimental

Crystal data

[Ho(n class="CellLine">C7H2NO5)(H2O)3]·H2O

M = 417.09

Monoclinic,

a = 9.879 (5) Å

b = 7.557 (4) Å

c = 15.386 (8) Å

β = 105.386 (5)°

V = 1107.5 (9) Å3

Z = 4

Mo Kα radiation

μ = 7.19 mm−1

T = 296 K

0.32 × 0.29 × 0.26 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2004 ▶) T min = 0.207, T max = 0.257

4776 measured reflections

2003 independent reflections

1646 reflections with I > 2σ(I)

R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.021

wR(F 2) = 0.047

S = 1.02

2003 reflections

196 parameters

12 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.71 e Å−3

Δρmin = −0.54 e Å−3

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); 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 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811016953/sj5136sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811016953/sj5136Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Ho(C7H2NO5)(H2O)3]·H2O	F(000) = 792
Mr = 417.09	Dx = 2.502 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2y/n	Cell parameters from 2292 reflections
a = 9.879 (5) Å	θ = 2.2–28.2°
b = 7.557 (4) Å	µ = 7.19 mm−1
c = 15.386 (8) Å	T = 296 K
β = 105.386 (5)°	Block, colorless
V = 1107.5 (9) Å3	0.32 × 0.29 × 0.26 mm
Z = 4

Bruker APEXII CCD diffractometer	2003 independent reflections
Radiation source: fine-focus sealed tube	1646 reflections with I > 2σ(I)
graphite	Rint = 0.025
φ and ω scans	θmax = 25.5°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −11→7
Tmin = 0.207, Tmax = 0.257	k = −8→9
4776 measured reflections	l = −16→17

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.021	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.047	w = 1/[σ2(Fo2) + (0.0176P)2] where P = (Fo2 + 2Fc2)/3
S = 1.02	(Δ/σ)max = 0.002
2003 reflections	Δρmax = 0.71 e Å−3
196 parameters	Δρmin = −0.54 e Å−3
12 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0119 (3)

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.

	x	y	z	Uiso*/Ueq
Ho1	0.501337 (17)	0.82185 (2)	0.747304 (11)	0.01332 (10)
C1	0.7829 (4)	0.5891 (5)	0.8379 (3)	0.0184 (9)
C2	0.7250 (4)	0.6133 (5)	0.9175 (3)	0.0158 (9)
C3	0.7940 (4)	0.5582 (5)	1.0018 (3)	0.0172 (9)
H3	0.8780	0.4963	1.0112	0.021*
C4	0.7379 (4)	0.5951 (5)	1.0743 (2)	0.0163 (9)
C5	0.6087 (4)	0.6828 (5)	1.0537 (3)	0.0193 (9)
H5	0.5652	0.7073	1.0991	0.023*
C6	0.5460 (4)	0.7328 (5)	0.9665 (3)	0.0157 (9)
C7	0.4083 (4)	0.8304 (5)	0.9374 (3)	0.0162 (9)
H1W	0.613 (6)	1.087 (8)	0.8854 (11)	0.08 (2)*
H2W	0.661 (5)	1.128 (7)	0.806 (3)	0.08 (2)*
H3W	0.332 (5)	0.547 (8)	0.7874 (18)	0.09 (2)*
H4W	0.313 (4)	0.523 (6)	0.6913 (15)	0.040 (15)*
H5W	0.484 (6)	0.5513 (17)	0.606 (4)	0.08 (2)*
H6W	0.524 (8)	0.714 (7)	0.569 (3)	0.12 (3)*
H7W	0.1510 (15)	0.841 (6)	0.945 (3)	0.057 (19)*
H8W	0.032 (5)	0.745 (8)	0.888 (4)	0.16 (4)*
N1	0.6032 (3)	0.7004 (4)	0.8981 (2)	0.0151 (7)
O1	0.7200 (3)	0.6723 (4)	0.76661 (19)	0.0274 (8)
O2	0.8899 (3)	0.4962 (4)	0.84514 (18)	0.0234 (7)
O3	0.3689 (3)	0.8732 (4)	0.85503 (18)	0.0201 (6)
O4	0.3418 (3)	0.8625 (4)	0.99379 (18)	0.0249 (7)
O5	0.8051 (3)	0.5493 (4)	1.15748 (17)	0.0200 (6)
O6	0.6030 (3)	1.0722 (4)	0.8286 (2)	0.0315 (8)
O7	0.3636 (3)	0.5656 (4)	0.7411 (2)	0.0295 (8)
O8	0.4963 (4)	0.6642 (4)	0.6113 (2)	0.0255 (7)
O9	0.0620 (4)	0.8221 (4)	0.9302 (3)	0.0392 (9)

	U11	U22	U33	U12	U13	U23
Ho1	0.01235 (13)	0.01734 (13)	0.01046 (14)	0.00009 (7)	0.00339 (8)	0.00057 (8)
C1	0.016 (2)	0.024 (2)	0.014 (2)	0.0019 (17)	0.0032 (17)	−0.0012 (17)
C2	0.015 (2)	0.018 (2)	0.014 (2)	0.0028 (16)	0.0033 (17)	−0.0011 (17)
C3	0.016 (2)	0.018 (2)	0.017 (2)	0.0040 (16)	0.0039 (17)	0.0012 (16)
C4	0.017 (2)	0.019 (2)	0.013 (2)	−0.0047 (16)	0.0028 (17)	0.0022 (17)
C5	0.019 (2)	0.022 (2)	0.019 (2)	−0.0011 (16)	0.0079 (18)	0.0022 (17)
C6	0.016 (2)	0.017 (2)	0.014 (2)	0.0005 (16)	0.0049 (17)	0.0004 (16)
C7	0.016 (2)	0.015 (2)	0.018 (2)	−0.0025 (15)	0.0059 (18)	−0.0032 (16)
N1	0.0145 (18)	0.0198 (19)	0.0126 (18)	0.0011 (13)	0.0063 (14)	0.0005 (13)
O1	0.0270 (17)	0.044 (2)	0.0138 (16)	0.0158 (14)	0.0108 (14)	0.0074 (13)
O2	0.0244 (17)	0.0273 (18)	0.0196 (16)	0.0151 (13)	0.0076 (13)	0.0013 (13)
O3	0.0150 (15)	0.0300 (17)	0.0150 (16)	0.0057 (12)	0.0033 (12)	0.0029 (12)
O4	0.0211 (16)	0.0410 (19)	0.0151 (16)	0.0065 (13)	0.0092 (13)	0.0003 (13)
O5	0.0158 (15)	0.0295 (17)	0.0124 (15)	−0.0036 (12)	−0.0005 (12)	0.0065 (12)
O6	0.036 (2)	0.041 (2)	0.021 (2)	−0.0177 (15)	0.0143 (16)	−0.0087 (15)
O7	0.0341 (19)	0.036 (2)	0.0202 (18)	−0.0165 (14)	0.0105 (16)	−0.0040 (15)
O8	0.036 (2)	0.0232 (19)	0.0186 (18)	−0.0012 (14)	0.0098 (15)	−0.0031 (13)
O9	0.027 (2)	0.029 (2)	0.059 (3)	−0.0001 (15)	0.0072 (19)	0.0033 (18)

Ho1—O5i	2.279 (3)	C5—C6	1.373 (5)
Ho1—O6	2.342 (3)	C5—H5	0.9300
Ho1—O7	2.354 (3)	C6—N1	1.341 (5)
Ho1—O1	2.386 (3)	C6—C7	1.508 (5)
Ho1—O2ii	2.393 (3)	C7—O4	1.243 (5)
Ho1—O8	2.397 (3)	C7—O3	1.265 (5)
Ho1—O3	2.400 (3)	O2—Ho1iii	2.393 (3)
Ho1—N1	2.450 (3)	O5—Ho1iv	2.279 (3)
C1—O2	1.249 (5)	O6—H1W	0.860 (10)
C1—O1	1.275 (5)	O6—H2W	0.858 (10)
C1—C2	1.493 (5)	O7—H3W	0.865 (10)
C2—N1	1.334 (5)	O7—H4W	0.861 (10)
C2—C3	1.361 (5)	O8—H5W	0.862 (10)
C3—C4	1.399 (5)	O8—H6W	0.861 (10)
C3—H3	0.9300	O9—H7W	0.860 (10)
C4—O5	1.322 (4)	O9—H8W	0.861 (10)
C4—C5	1.398 (5)
O5i—Ho1—O6	98.86 (11)	C3—C2—C1	122.7 (3)
O5i—Ho1—O7	86.39 (12)	C2—C3—C4	119.7 (4)
O6—Ho1—O7	147.96 (12)	C2—C3—H3	120.2
O5i—Ho1—O1	150.97 (10)	C4—C3—H3	120.2
O6—Ho1—O1	94.04 (12)	O5—C4—C5	122.5 (4)
O7—Ho1—O1	96.31 (12)	O5—C4—C3	121.1 (4)
O5i—Ho1—O2ii	81.27 (10)	C5—C4—C3	116.5 (4)
O6—Ho1—O2ii	71.09 (11)	C6—C5—C4	119.9 (4)
O7—Ho1—O2ii	140.78 (10)	C6—C5—H5	120.0
O1—Ho1—O2ii	78.49 (10)	C4—C5—H5	120.0
O5i—Ho1—O8	82.29 (11)	N1—C6—C5	122.8 (4)
O6—Ho1—O8	140.74 (12)	N1—C6—C7	113.0 (3)
O7—Ho1—O8	71.19 (12)	C5—C6—C7	124.2 (4)
O1—Ho1—O8	71.43 (11)	O4—C7—O3	124.8 (4)
O2ii—Ho1—O8	70.33 (11)	O4—C7—C6	119.4 (4)
O5i—Ho1—O3	79.50 (10)	O3—C7—C6	115.8 (3)
O6—Ho1—O3	74.68 (11)	C2—N1—C6	117.2 (3)
O7—Ho1—O3	75.28 (11)	C2—N1—Ho1	121.0 (3)
O1—Ho1—O3	129.20 (9)	C6—N1—Ho1	121.4 (2)
O2ii—Ho1—O3	137.27 (9)	C1—O1—Ho1	124.0 (2)
O8—Ho1—O3	142.60 (11)	C1—O2—Ho1iii	139.4 (3)
O5i—Ho1—N1	143.51 (10)	C7—O3—Ho1	124.8 (2)
O6—Ho1—N1	77.69 (12)	C4—O5—Ho1iv	127.1 (2)
O7—Ho1—N1	79.53 (11)	Ho1—O6—H1W	124 (3)
O1—Ho1—N1	64.77 (10)	Ho1—O6—H2W	115 (3)
O2ii—Ho1—N1	129.28 (10)	H1W—O6—H2W	116 (2)
O8—Ho1—N1	123.29 (11)	Ho1—O7—H3W	116 (3)
O3—Ho1—N1	64.44 (10)	Ho1—O7—H4W	123 (3)
O2—C1—O1	124.2 (4)	H3W—O7—H4W	114.8 (19)
O2—C1—C2	119.7 (3)	Ho1—O8—H5W	123 (3)
O1—C1—C2	116.1 (3)	Ho1—O8—H6W	120 (4)
N1—C2—C3	123.9 (4)	H5W—O8—H6W	115.3 (19)
N1—C2—C1	113.4 (3)	H7W—O9—H8W	116 (2)
O2—C1—C2—N1	−173.7 (4)	O3—Ho1—N1—C2	−179.5 (3)
O1—C1—C2—N1	8.7 (5)	O5i—Ho1—N1—C6	−15.3 (4)
O2—C1—C2—C3	9.1 (6)	O6—Ho1—N1—C6	72.9 (3)
O1—C1—C2—C3	−168.6 (4)	O7—Ho1—N1—C6	−84.4 (3)
N1—C2—C3—C4	−1.0 (6)	O1—Ho1—N1—C6	173.5 (3)
C1—C2—C3—C4	175.9 (4)	O2ii—Ho1—N1—C6	125.6 (3)
C2—C3—C4—O5	−177.4 (4)	O8—Ho1—N1—C6	−143.5 (3)
C2—C3—C4—C5	2.3 (6)	O3—Ho1—N1—C6	−5.8 (3)
O5—C4—C5—C6	177.7 (4)	O2—C1—O1—Ho1	172.6 (3)
C3—C4—C5—C6	−2.0 (6)	C2—C1—O1—Ho1	−9.9 (5)
C4—C5—C6—N1	0.3 (6)	O5i—Ho1—O1—C1	−163.5 (3)
C4—C5—C6—C7	−178.9 (4)	O6—Ho1—O1—C1	80.1 (3)
N1—C6—C7—O4	177.2 (3)	O7—Ho1—O1—C1	−69.5 (3)
C5—C6—C7—O4	−3.4 (6)	O2ii—Ho1—O1—C1	149.8 (3)
N1—C6—C7—O3	−2.4 (5)	O8—Ho1—O1—C1	−137.3 (3)
C5—C6—C7—O3	176.9 (4)	O3—Ho1—O1—C1	6.6 (4)
C3—C2—N1—C6	−0.8 (6)	N1—Ho1—O1—C1	5.7 (3)
C1—C2—N1—C6	−178.0 (3)	O1—C1—O2—Ho1iii	−28.4 (7)
C3—C2—N1—Ho1	173.2 (3)	C2—C1—O2—Ho1iii	154.1 (3)
C1—C2—N1—Ho1	−4.0 (5)	O4—C7—O3—Ho1	177.4 (3)
C5—C6—N1—C2	1.1 (6)	C6—C7—O3—Ho1	−3.0 (5)
C7—C6—N1—C2	−179.6 (3)	O5i—Ho1—O3—C7	178.8 (3)
C5—C6—N1—Ho1	−172.8 (3)	O6—Ho1—O3—C7	−78.9 (3)
C7—C6—N1—Ho1	6.5 (4)	O7—Ho1—O3—C7	89.8 (3)
O5i—Ho1—N1—C2	171.0 (3)	O1—Ho1—O3—C7	3.6 (3)
O6—Ho1—N1—C2	−100.7 (3)	O2ii—Ho1—O3—C7	−116.6 (3)
O7—Ho1—N1—C2	101.9 (3)	O8—Ho1—O3—C7	116.6 (3)
O1—Ho1—N1—C2	−0.2 (3)	N1—Ho1—O3—C7	4.5 (3)
O2ii—Ho1—N1—C2	−48.1 (3)	C5—C4—O5—Ho1iv	−106.4 (4)
O8—Ho1—N1—C2	42.8 (3)	C3—C4—O5—Ho1iv	73.3 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O9—H8W···O2v	0.86 (1)	2.33 (4)	3.080 (5)	145 (6)
O9—H7W···O4	0.86 (1)	1.84 (1)	2.693 (5)	170 (5)
O8—H6W···O9vi	0.86 (1)	2.28 (3)	3.026 (5)	145 (5)
O8—H5W···O9vii	0.86 (1)	1.84 (2)	2.689 (5)	168 (5)
O7—H4W···O3vii	0.86 (1)	2.08 (3)	2.788 (4)	139 (4)
O7—H3W···O5viii	0.87 (1)	1.92 (3)	2.711 (4)	152 (4)
O6—H2W···O1ii	0.86 (1)	1.85 (2)	2.671 (4)	159 (5)
O6—H1W···O4ix	0.86 (1)	1.83 (1)	2.687 (4)	171 (5)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O9—H8W⋯O2i	0.86 (1)	2.33 (4)	3.080 (5)	145 (6)
O9—H7W⋯O4	0.86 (1)	1.84 (1)	2.693 (5)	170 (5)
O8—H6W⋯O9ii	0.86 (1)	2.28 (3)	3.026 (5)	145 (5)
O8—H5W⋯O9iii	0.86 (1)	1.84 (2)	2.689 (5)	168 (5)
O7—H4W⋯O3iii	0.86 (1)	2.08 (3)	2.788 (4)	139 (4)
O7—H3W⋯O5iv	0.87 (1)	1.92 (3)	2.711 (4)	152 (4)
O6—H2W⋯O1v	0.86 (1)	1.85 (2)	2.671 (4)	159 (5)
O6—H1W⋯O4vi	0.86 (1)	1.83 (1)	2.687 (4)	171 (5)

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