Poly[[triaqua­(μ3-4-oxidopyridine-2,6-dicarboxyl­ato)holmium(III)] mono­hydrate]

Gao, Z.-Q.; Lv, D.-Y.; Gu, J.-Z.; Li, H.-J.

doi:10.1107/S1600536811016953

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 6| June 2011| Page m740

doi:10.1107/S1600536811016953

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Poly[[triaqua(μ₃-4-oxidopyridine-2,6-dicarboxylato)holmium(III)] monohydrate]

Zhu-Qing Gao,^a ^* Dong-Yu Lv,^b Jin-Zhong Gu ^b and Hong-Jin Li ^a

^aSchool of Chemistry and Biological Engineering, Taiyuan University of Science and Technology, Taiyuan 030021, People's Republic of China, and ^bKey Laboratory of Nonferrous Metal Chemistry and Resources Utilization of Gansu Province, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000, People's Republic of China
^*Correspondence e-mail: zqgao2008@163.com

(Received 28 April 2011; accepted 5 May 2011; online 11 May 2011)

In the title coordination polymer, {[Ho(C₇H₂NO₅)(H₂O)₃]·H₂O}_n, the Ho^III atom is eight-coordinated by a tridentate 4-oxidopyridine-2,6-dicarboxylate trianion, two monodentate anions and three water molecules, forming a distorted bicapped trigonal–prismatic HoNO₇ 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 molecules generate a three-dimensional supramolecular 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 Ho^III, see: Wang et al. (2007); Munoz et al. (2005 ).

Experimental

Crystal data

[Ho(C₇H₂NO₅)(H₂O)₃]·H₂O
M_r = 417.09
Monoclinic, P 2₁ /n
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[F² > 2σ(F²)] = 0.021
wR(F²) = 0.047
S = 1.02
2003 reflections
196 parameters
12 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.71 e Å⁻³
Δρ_min = −0.54 e Å⁻³

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⋯O5^iv	0.87 (1)	1.92 (3)	2.711 (4)	152 (4)
O6—H2W⋯O1^v	0.86 (1)	1.85 (2)	2.671 (4)	159 (5)
O6—H1W⋯O4^vi	0.86 (1)	1.83 (1)	2.687 (4)	171 (5)
Symmetry codes: (i) x-1, y, z; (ii) $[x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (iii) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iv) -x+1, -y+1, -z+2; (v) $[-x+{\script{3\over 2}}, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (vi) -x+1, -y+2, -z+2.

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.

Supporting information

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

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

checkCIF report

Comment top

Lanthanide coordination polymers have shown not only versatile architectures but also desirable properties, e.g., luminescent, magnetic, catalytic, and gas absorption and separation properties (Wang et al., 2007; Lv et al., 2010). In order to extend our investigations in this field, we designed and synthesized one lanthanide coordination polymer {[Ho(C₇H₂NO₅)(H₂O)₃].H₂O}_n by choosing 4-oxidopyridine-2,6-dicarboxylicacid as a functional ligand, and report its structure here.

The title compound is isotypic with its Dy (Gao et al., 2006) and Eu (Lv et al., 2010) analogues. As shown in Fig.1, the asymmetric unit of the cell contains one Ho(III) ion, one 4-oxidopyridine-2,6-dicarboxylate anion, three coordinated water molecules, and one water molecule of crystallization. The Ho atom is eight-coordinated by seven oxygen atoms from three anions and three coordinated water molecules and by one nitrogen atom from one tridentate anion (the other two anions are monodentate), forming a distorted bicapped trigonal-prismatic coordination environment.

Important bond distances are presented in Table 1. The Ho–O bond lengths [2.279 (3) to 2.400 (3) Å] are shorter than the Ho–N bond length [2.450 (3) Å], which is in agreement with the bond lengths observed in other Ho(III) complexes (Wang et al., 2007; Munoz et al., 2005). The anion adopts a µ₃-pentadentate coordination mode, as shown in Fig.1. The anions bridge the adjacent Ho^III ions to form infinite double chains (Fig.2). Adjacent chains are further connected by the coordination of the anions and Ho(III) ions into a two-dimensional sheet (Fig.3), which are further extended into a three-dimensional supramolecular framework through O–H···O hydrogen-bonding interactions including both coordinated and uncoordinated water molecules (Table 2).

Related literature top

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 eight-coordinate Ho^III complexes, see: Wang et al. (2007); Munoz et al. (2005).

Experimental top

To a solution of holmium(III)nitrate hexahydrate (0.138 g, 0.3 mmol) in water (5 ml) was added an aqueous solution (5 ml) of the ligand (0.060 g, 0.3 mmol) and a drop of triethylamine. The reactants were sealed in a 25-ml Teflon-lined, stainless-steel Parr bomb. The bomb was heated at 433 K for 3 days. The cool solution yielded colorless single crystals in ca 75% yield. Anal. Calcd for C₇H₁₀TbNO₉: C, 20.16; H, 2.42; N, 3.36. Found: C, 20.45; H, 2.17; N, 3.64.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); 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 (Sheldrick, 2008).

Figures top

	Fig. 1. The asymmetric unit of the title complex, showing the atom-labeling scheme. Displacement ellipsoids are drawn at the 30% probability level.
	Fig. 2. View along the b axis, showing the polymeric double chain.
	Fig. 3. View along the a axis, showing the sheet structure of {[Ho(C₇H₂NO₅)(H₂O)₃].H₂O}_n.

Poly[[triaqua(µ₃-4-oxidopyridine-2,6-dicarboxylato)holmium(III)] monohydrate] top

Crystal data top

[Ho(C₇H₂NO₅)(H₂O)₃]·H₂O	F(000) = 792
M_r = 417.09	D_x = 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

Data collection top

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

Refinement top

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(F_o²) + (0.0176P)²] where P = (F_o² + 2F_c²)/3
S = 1.02	(Δ/σ)_max = 0.002
2003 reflections	Δρ_max = 0.71 e Å⁻³
196 parameters	Δρ_min = −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)

Crystal data top

[Ho(C₇H₂NO₅)(H₂O)₃]·H₂O	V = 1107.5 (9) Å³
M_r = 417.09	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 9.879 (5) Å	µ = 7.19 mm⁻¹
b = 7.557 (4) Å	T = 296 K
c = 15.386 (8) Å	0.32 × 0.29 × 0.26 mm
β = 105.386 (5)°

Data collection top

Bruker APEXII CCD diffractometer	2003 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2004)	1646 reflections with I > 2σ(I)
T_min = 0.207, T_max = 0.257	R_int = 0.025
4776 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.021	12 restraints
wR(F²) = 0.047	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	Δρ_max = 0.71 e Å⁻³
2003 reflections	Δρ_min = −0.54 e Å⁻³
196 parameters

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq
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)

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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—Ho1^iv	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—Ho1^iv	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—Ho1^iv	−106.4 (4)
O8—Ho1—N1—C2	42.8 (3)	C3—C4—O5—Ho1^iv	73.3 (4)

Symmetry codes: (i) x−1/2, −y+3/2, z−1/2; (ii) −x+3/2, y+1/2, −z+3/2; (iii) −x+3/2, y−1/2, −z+3/2; (iv) x+1/2, −y+3/2, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O9—H8W···O2^v	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···O9^vi	0.86 (1)	2.28 (3)	3.026 (5)	145 (5)
O8—H5W···O9^vii	0.86 (1)	1.84 (2)	2.689 (5)	168 (5)
O7—H4W···O3^vii	0.86 (1)	2.08 (3)	2.788 (4)	139 (4)
O7—H3W···O5^viii	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···O4^ix	0.86 (1)	1.83 (1)	2.687 (4)	171 (5)

Symmetry codes: (ii) −x+3/2, y+1/2, −z+3/2; (v) x−1, y, z; (vi) x+1/2, −y+3/2, z−1/2; (vii) −x+1/2, y−1/2, −z+3/2; (viii) −x+1, −y+1, −z+2; (ix) −x+1, −y+2, −z+2.

Experimental details

Crystal data
Chemical formula	[Ho(C₇H₂NO₅)(H₂O)₃]·H₂O
M_r	417.09
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	296
a, b, c (Å)	9.879 (5), 7.557 (4), 15.386 (8)
β (°)	105.386 (5)
V (Å³)	1107.5 (9)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	7.19
Crystal size (mm)	0.32 × 0.29 × 0.26

Data collection
Diffractometer	Bruker APEXII CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2004)
T_min, T_max	0.207, 0.257
No. of measured, independent and observed [I > 2σ(I)] reflections	4776, 2003, 1646
R_int	0.025
(sin θ/λ)_max (Å⁻¹)	0.606

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.021, 0.047, 1.02
No. of reflections	2003
No. of parameters	196
No. of restraints	12
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.71, −0.54

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O9—H8W···O2ⁱ	0.861 (10)	2.33 (4)	3.080 (5)	145 (6)
O9—H7W···O4	0.860 (10)	1.842 (14)	2.693 (5)	170 (5)
O8—H6W···O9ⁱⁱ	0.861 (10)	2.28 (3)	3.026 (5)	145 (5)
O8—H5W···O9ⁱⁱⁱ	0.862 (10)	1.841 (17)	2.689 (5)	168 (5)
O7—H4W···O3ⁱⁱⁱ	0.861 (10)	2.08 (3)	2.788 (4)	139 (4)
O7—H3W···O5^iv	0.865 (10)	1.92 (3)	2.711 (4)	152 (4)
O6—H2W···O1^v	0.858 (10)	1.85 (2)	2.671 (4)	159 (5)
O6—H1W···O4^vi	0.860 (10)	1.834 (14)	2.687 (4)	171 (5)

Symmetry codes: (i) x−1, y, z; (ii) x+1/2, −y+3/2, z−1/2; (iii) −x+1/2, y−1/2, −z+3/2; (iv) −x+1, −y+1, −z+2; (v) −x+3/2, y+1/2, −z+3/2; (vi) −x+1, −y+2, −z+2.

References

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