Bis(μ-4-hydroxy­benzoato-κ2O:O′)bis­[triaqua­bis(4-hydroxy­benzoato)-κO;κ2O,O′-terbium(III)] deca­hydrate

Zhu, Y.-M.; Feng, P.-P.; Yang, Y.-Y.; Ng, S.W.

doi:10.1107/S1600536809052489

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 1| January 2010| Pages m54-m55

doi:10.1107/S1600536809052489

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Bis(μ-4-hydroxybenzoato-κ²O:O′)bis[triaquabis(4-hydroxybenzoato)-κO;κ²O,O′-terbium(III)] decahydrate

Yi-Min Zhu,^a Pei-Pei Feng,^a Yang-Yi Yang ^a and Seik Weng Ng ^b ^*

^aMOE Key Laboratory of Bioinorganic and Synthetic Chemistry, School of Chemistry & Chemical Engineering, Sun Yat-Sen University, Guangzhou 510275, People's Republic of China, and ^bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
^*Correspondence e-mail: seikweng@um.edu.my

(Received 6 December 2009; accepted 7 December 2009; online 12 December 2009)

The title dinuclear compound, [Tb₂(C₇H₅O₃)₆(H₂O)₆]·10H₂O, lies on a center of inversion and the two Tb^III atoms are bridged by two 4-hydroxybenzoate anions; each metal atom is further coordinated by one monodentate anion and chelated by the third anion. The eight-coordinate geometry approximates a square antiprism. Hydrogen bonds of the O—H⋯O type connect the uncoordinated water molecules to the dinuclear species, forming a three-dimensional network.

Related literature

For a related structure, Tb₂(H₂O)₂(DMF)₂(C₇H₅O₃)₆, see: Zhou et al. (2008 ).

Experimental

Crystal data

[Tb₂(C₇H₅O₃)₆(H₂O)₆]·10H₂O
M_r = 1428.76
Triclinic, $[P \overline 1]$
a = 10.8308 (5) Å
b = 11.3337 (6) Å
c = 11.5128 (6) Å
α = 90.463 (1)°
β = 101.690 (1)°
γ = 105.249 (1)°
V = 1332.37 (12) Å³
Z = 1
Mo Kα radiation
μ = 2.73 mm⁻¹
T = 173 K
0.47 × 0.30 × 0.19 mm

Data collection

Bruker SMART area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.360, T_max = 0.625
12836 measured reflections
5756 independent reflections
5391 reflections with I > 2σ(I)
R_int = 0.018

Refinement

R[F² > 2σ(F²)] = 0.018
wR(F²) = 0.059
S = 1.09
5756 reflections
409 parameters
27 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.67 e Å⁻³
Δρ_min = −0.64 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H3⋯O7wⁱ	0.84 (1)	1.82 (2)	2.612 (3)	158 (3)
O6—H6⋯O6wⁱⁱ	0.83 (1)	1.87 (1)	2.678 (3)	165 (4)
O9—H9⋯O4wⁱⁱⁱ	0.84 (1)	1.98 (2)	2.763 (3)	156 (3)
O1w—H11⋯O4w	0.84 (1)	2.04 (1)	2.870 (3)	171 (3)
O1w—H12⋯O9^iv	0.83 (1)	1.96 (1)	2.766 (3)	164 (3)
O2w—H22⋯O5w	0.83 (1)	1.86 (1)	2.678 (3)	167 (3)
O2w—H21⋯O5w^v	0.84 (1)	2.20 (2)	2.952 (3)	150 (3)
O3w—H31⋯O3ⁱⁱ	0.84 (1)	1.95 (1)	2.777 (3)	171 (3)
O3w—H32⋯O7^vi	0.84 (1)	2.25 (2)	2.916 (2)	137 (3)
O4w—H41⋯O8w^vii	0.84 (1)	1.94 (1)	2.753 (3)	163 (3)
O4w—H42⋯O5^viii	0.84 (1)	2.10 (1)	2.927 (3)	169 (3)
O5w—H52⋯O7w	0.85 (1)	2.01 (2)	2.811 (3)	157 (3)
O5w—H51⋯O8w^ix	0.86 (1)	1.96 (1)	2.791 (3)	163 (3)
O6w—H61⋯O2	0.85 (1)	1.90 (1)	2.743 (2)	172 (3)
O6w—H62⋯O5	0.84 (1)	1.95 (1)	2.785 (2)	171 (3)
O7w—H71⋯O6w	0.84 (1)	1.90 (1)	2.732 (3)	172 (3)
O7w—H72⋯O5^x	0.83 (1)	1.89 (1)	2.725 (3)	175 (3)
O8w—H81⋯O1^xi	0.84 (1)	2.10 (2)	2.818 (3)	144 (3)
O8w—H82⋯O6	0.84 (1)	1.90 (1)	2.713 (3)	164 (3)
Symmetry codes: (i) -x+2, -y+1, -z; (ii) x-1, y, z; (iii) x+1, y+1, z; (iv) -x+2, -y+1, -z+1; (v) -x+1, -y+1, -z; (vi) -x+1, -y+1, -z+1; (vii) -x, -y, -z+1; (viii) -x+1, -y, -z+1; (ix) -x, -y, -z; (x) -x+1, -y, -z; (xi) x-1, y-1, z.

Data collection: SMART (Bruker, 2001 ); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001 ); software used to prepare material for publication: publCIF (Westrip, 2009 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809052489/xu2706sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809052489/xu2706Isup2.hkl

checkCIF report

Related literature top

For a related structure, Tb₂(H₂O)₂(DMF)₂(C₇H₅O₃)₆, see: Zhou et al. (2008).

Experimental top

4-Hydroxybenzoic acid (0.3 mmol) and sodium hydroxide (0.3 mmol) were dissolved in water (5 ml) and this was mixed with a solution of terbium chloride (0.1 mmol) dissolved in water (5 ml). The white precipitate that formed was removed by filtration. Colorless crystals were isolated from the filtrated after two weeks.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2009).

Figures top

	Fig. 1. Thermal ellipsoid plot (Barbour, 2001) of Tb₂(H₂O)₆(C₇H₅O₃)₆^.10H₂O at the 70% probability level; hydrogen atoms are drawn as sphere of arbitrary radius.
	Fig. 2. Detail of the coordination environment of the terbium(III) atom.

Bis(µ-4-hydroxybenzoato-κ²O:O')bis[triaquabis(4- hydroxybenzoato)-κO;κ²O,O'-terbium(III)] decahydrate top

Crystal data top

[Tb₂(C₇H₅O₃)₆(H₂O)₆]·10H₂O	Z = 1
M_r = 1428.76	F(000) = 716
Triclinic, P1	D_x = 1.781 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.8308 (5) Å	Cell parameters from 5392 reflections
b = 11.3337 (6) Å	θ = 2.3–27.0°
c = 11.5128 (6) Å	µ = 2.73 mm⁻¹
α = 90.463 (1)°	T = 173 K
β = 101.690 (1)°	Block, colorless
γ = 105.249 (1)°	0.47 × 0.30 × 0.19 mm
V = 1332.37 (12) Å³

Data collection top

Bruker SMART area-detector diffractometer	5756 independent reflections
Radiation source: fine-focus sealed tube	5391 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.018
ϕ and ω scans	θ_max = 27.0°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −13→13
T_min = 0.360, T_max = 0.625	k = −13→14
12836 measured reflections	l = −14→14

Refinement top

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)] = 0.018	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.059	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	w = 1/[σ²(F_o²) + (0.0407P)² + 0.0925P] where P = (F_o² + 2F_c²)/3
5756 reflections	(Δ/σ)_max = 0.001
409 parameters	Δρ_max = 0.67 e Å⁻³
27 restraints	Δρ_min = −0.64 e Å⁻³

Crystal data top

[Tb₂(C₇H₅O₃)₆(H₂O)₆]·10H₂O	γ = 105.249 (1)°
M_r = 1428.76	V = 1332.37 (12) Å³
Triclinic, P1	Z = 1
a = 10.8308 (5) Å	Mo Kα radiation
b = 11.3337 (6) Å	µ = 2.73 mm⁻¹
c = 11.5128 (6) Å	T = 173 K
α = 90.463 (1)°	0.47 × 0.30 × 0.19 mm
β = 101.690 (1)°

Data collection top

Bruker SMART area-detector diffractometer	5756 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	5391 reflections with I > 2σ(I)
T_min = 0.360, T_max = 0.625	R_int = 0.018
12836 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.018	27 restraints
wR(F²) = 0.059	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	Δρ_max = 0.67 e Å⁻³
5756 reflections	Δρ_min = −0.64 e Å⁻³
409 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Tb1	0.521099 (9)	0.392335 (9)	0.316629 (8)	0.01393 (5)
O1	0.68247 (16)	0.52500 (16)	0.22113 (15)	0.0219 (4)
O2	0.71938 (16)	0.35118 (15)	0.28025 (15)	0.0189 (3)
O3	1.25530 (17)	0.60503 (18)	0.13235 (17)	0.0243 (4)
H3	1.262 (3)	0.6687 (19)	0.095 (3)	0.036*
O4	0.44616 (17)	0.20553 (16)	0.21445 (16)	0.0233 (4)
O5	0.44536 (17)	0.00991 (16)	0.21119 (16)	0.0236 (4)
O6	−0.15974 (18)	−0.03603 (17)	0.16884 (18)	0.0280 (4)
H6	−0.192 (3)	0.023 (2)	0.171 (3)	0.042*
O7	0.66267 (16)	0.51402 (16)	0.47709 (14)	0.0207 (3)
O8	0.65933 (16)	0.66801 (16)	0.59555 (15)	0.0209 (4)
O9	1.23480 (17)	0.85877 (17)	0.50180 (16)	0.0220 (4)
H9	1.262 (3)	0.9320 (13)	0.529 (3)	0.033*
O1w	0.56576 (17)	0.25542 (17)	0.47360 (16)	0.0241 (4)
H11	0.509 (2)	0.206 (2)	0.502 (3)	0.036*
H12	0.6353 (16)	0.234 (3)	0.487 (3)	0.036*
O2w	0.40382 (18)	0.41807 (17)	0.12181 (15)	0.0233 (4)
H21	0.405 (3)	0.4895 (13)	0.102 (2)	0.035*
H22	0.426 (3)	0.380 (2)	0.071 (2)	0.035*
O3w	0.44922 (17)	0.57723 (16)	0.32029 (15)	0.0201 (3)
H31	0.397 (2)	0.593 (3)	0.2625 (14)	0.030*
H32	0.428 (3)	0.593 (3)	0.3838 (13)	0.030*
O4w	0.39635 (19)	0.08545 (18)	0.59456 (16)	0.0267 (4)
H41	0.358 (3)	0.130 (3)	0.624 (2)	0.040*
H42	0.450 (3)	0.066 (3)	0.6490 (19)	0.040*
O5w	0.4872 (2)	0.3305 (2)	−0.05591 (17)	0.0309 (4)
H51	0.421 (2)	0.294 (3)	−0.111 (2)	0.046*
H52	0.530 (3)	0.278 (2)	−0.037 (3)	0.046*
O6w	0.69870 (17)	0.12258 (17)	0.18465 (16)	0.0235 (4)
H61	0.711 (3)	0.1957 (12)	0.211 (3)	0.035*
H62	0.6246 (17)	0.082 (2)	0.194 (3)	0.035*
O7w	0.6606 (2)	0.18314 (17)	−0.04660 (16)	0.0286 (4)
H71	0.676 (3)	0.160 (3)	0.0230 (11)	0.043*
H72	0.627 (3)	0.1215 (18)	−0.0936 (19)	0.043*
O8w	−0.30680 (19)	−0.22701 (18)	0.26414 (18)	0.0301 (4)
H81	−0.280 (3)	−0.2897 (17)	0.276 (3)	0.045*
H82	−0.249 (2)	−0.172 (2)	0.242 (3)	0.045*
C1	0.7539 (2)	0.4523 (2)	0.2315 (2)	0.0169 (5)
C2	0.8802 (2)	0.4855 (2)	0.19285 (19)	0.0163 (4)
C3	0.9139 (2)	0.5908 (2)	0.1316 (2)	0.0190 (5)
H3A	0.8513	0.6352	0.1057	0.023*
C4	1.0383 (2)	0.6307 (2)	0.1084 (2)	0.0186 (5)
H4	1.0609	0.7020	0.0660	0.022*
C5	1.1296 (2)	0.5662 (2)	0.1474 (2)	0.0177 (5)
C6	1.0956 (2)	0.4574 (2)	0.2042 (2)	0.0188 (5)
H6A	1.1572	0.4112	0.2268	0.023*
C7	0.9713 (2)	0.4181 (2)	0.22698 (19)	0.0178 (5)
H7	0.9475	0.3446	0.2661	0.021*
C8	0.3871 (2)	0.0935 (2)	0.2068 (2)	0.0184 (5)
C9	0.2416 (2)	0.0589 (2)	0.1919 (2)	0.0168 (4)
C10	0.1763 (2)	−0.0536 (2)	0.2258 (2)	0.0206 (5)
H10	0.2237	−0.1109	0.2542	0.025*
C11	0.0414 (2)	−0.0831 (2)	0.2184 (2)	0.0224 (5)
H11A	−0.0027	−0.1592	0.2440	0.027*
C12	−0.0276 (2)	−0.0015 (2)	0.1740 (2)	0.0201 (5)
C13	0.0352 (2)	0.1103 (2)	0.1364 (2)	0.0214 (5)
H13	−0.0135	0.1651	0.1034	0.026*
C14	0.1704 (2)	0.1410 (2)	0.1477 (2)	0.0207 (5)
H14	0.2146	0.2185	0.1251	0.025*
C15	0.7152 (2)	0.6180 (2)	0.53115 (19)	0.0159 (4)
C16	0.8513 (2)	0.6851 (2)	0.52099 (19)	0.0153 (4)
C17	0.9058 (2)	0.8072 (2)	0.56448 (19)	0.0167 (4)
H17	0.8550	0.8494	0.5982	0.020*
C18	1.0337 (2)	0.8673 (2)	0.5587 (2)	0.0187 (5)
H18	1.0704	0.9503	0.5883	0.022*
C19	1.1080 (2)	0.8052 (2)	0.5093 (2)	0.0177 (5)
C20	1.0543 (2)	0.6841 (2)	0.4635 (2)	0.0187 (5)
H20	1.1045	0.6427	0.4282	0.022*
C21	0.9260 (2)	0.6245 (2)	0.4702 (2)	0.0176 (5)
H21A	0.8890	0.5418	0.4398	0.021*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Tb1	0.01190 (7)	0.01180 (7)	0.01807 (7)	0.00220 (4)	0.00446 (4)	0.00005 (4)
O1	0.0188 (8)	0.0190 (9)	0.0318 (9)	0.0082 (7)	0.0104 (7)	0.0067 (7)
O2	0.0174 (8)	0.0138 (8)	0.0276 (8)	0.0042 (6)	0.0098 (6)	0.0035 (6)
O3	0.0152 (8)	0.0248 (10)	0.0348 (10)	0.0051 (7)	0.0099 (7)	0.0120 (8)
O4	0.0198 (8)	0.0152 (9)	0.0338 (9)	0.0032 (7)	0.0051 (7)	−0.0029 (7)
O5	0.0186 (8)	0.0183 (9)	0.0343 (9)	0.0062 (7)	0.0049 (7)	−0.0008 (7)
O6	0.0173 (9)	0.0201 (10)	0.0484 (11)	0.0055 (7)	0.0105 (8)	0.0042 (8)
O7	0.0160 (8)	0.0188 (9)	0.0244 (8)	0.0005 (7)	0.0032 (6)	−0.0025 (7)
O8	0.0174 (8)	0.0170 (9)	0.0302 (9)	0.0039 (7)	0.0105 (7)	−0.0001 (7)
O9	0.0134 (8)	0.0204 (9)	0.0321 (9)	0.0023 (7)	0.0079 (7)	0.0027 (7)
O1w	0.0184 (8)	0.0241 (10)	0.0337 (9)	0.0082 (7)	0.0108 (7)	0.0114 (7)
O2w	0.0316 (10)	0.0196 (9)	0.0203 (8)	0.0097 (8)	0.0058 (7)	0.0005 (7)
O3w	0.0237 (9)	0.0198 (9)	0.0195 (8)	0.0093 (7)	0.0065 (7)	0.0013 (7)
O4w	0.0262 (10)	0.0251 (10)	0.0301 (9)	0.0082 (8)	0.0067 (7)	0.0042 (8)
O5w	0.0298 (10)	0.0359 (12)	0.0292 (10)	0.0122 (9)	0.0072 (8)	−0.0007 (8)
O6w	0.0200 (9)	0.0194 (9)	0.0330 (10)	0.0057 (7)	0.0092 (7)	0.0001 (7)
O7w	0.0404 (11)	0.0183 (9)	0.0272 (9)	0.0055 (8)	0.0109 (8)	0.0021 (7)
O8w	0.0293 (10)	0.0204 (10)	0.0427 (11)	0.0062 (8)	0.0128 (8)	0.0068 (8)
C1	0.0153 (11)	0.0168 (11)	0.0172 (10)	0.0023 (9)	0.0030 (8)	−0.0022 (9)
C2	0.0156 (10)	0.0159 (11)	0.0170 (10)	0.0029 (9)	0.0047 (8)	0.0000 (8)
C3	0.0185 (11)	0.0181 (12)	0.0224 (11)	0.0074 (9)	0.0057 (9)	0.0039 (9)
C4	0.0207 (11)	0.0155 (11)	0.0206 (11)	0.0047 (9)	0.0066 (9)	0.0040 (9)
C5	0.0162 (11)	0.0183 (12)	0.0185 (11)	0.0028 (9)	0.0057 (8)	−0.0004 (9)
C6	0.0180 (11)	0.0180 (12)	0.0222 (11)	0.0066 (9)	0.0055 (9)	0.0046 (9)
C7	0.0190 (11)	0.0155 (11)	0.0182 (10)	0.0028 (9)	0.0046 (8)	0.0029 (9)
C8	0.0181 (11)	0.0172 (12)	0.0189 (10)	0.0026 (9)	0.0044 (8)	−0.0012 (9)
C9	0.0185 (11)	0.0136 (11)	0.0185 (10)	0.0046 (9)	0.0039 (8)	−0.0004 (8)
C10	0.0203 (11)	0.0158 (12)	0.0276 (12)	0.0078 (9)	0.0054 (9)	0.0029 (9)
C11	0.0222 (12)	0.0147 (12)	0.0318 (13)	0.0040 (10)	0.0102 (10)	0.0027 (10)
C12	0.0186 (11)	0.0184 (12)	0.0230 (11)	0.0036 (9)	0.0055 (9)	−0.0021 (9)
C13	0.0215 (12)	0.0185 (12)	0.0247 (12)	0.0082 (10)	0.0023 (9)	0.0034 (9)
C14	0.0216 (12)	0.0156 (12)	0.0245 (11)	0.0032 (10)	0.0064 (9)	0.0022 (9)
C15	0.0141 (10)	0.0166 (11)	0.0176 (10)	0.0052 (9)	0.0031 (8)	0.0036 (8)
C16	0.0147 (10)	0.0166 (11)	0.0142 (10)	0.0043 (9)	0.0021 (8)	0.0016 (8)
C17	0.0163 (11)	0.0163 (11)	0.0189 (10)	0.0055 (9)	0.0051 (8)	0.0024 (9)
C18	0.0188 (11)	0.0148 (11)	0.0221 (11)	0.0030 (9)	0.0053 (9)	0.0008 (9)
C19	0.0121 (10)	0.0209 (12)	0.0200 (11)	0.0036 (9)	0.0040 (8)	0.0051 (9)
C20	0.0175 (11)	0.0190 (12)	0.0217 (11)	0.0070 (9)	0.0064 (9)	0.0001 (9)
C21	0.0163 (11)	0.0161 (11)	0.0189 (10)	0.0026 (9)	0.0028 (8)	−0.0008 (9)

Geometric parameters (Å, º) top

Tb1—O4	2.2791 (17)	O8w—H81	0.836 (10)
Tb1—O7	2.3162 (16)	O8w—H82	0.840 (10)
Tb1—O8ⁱ	2.3276 (16)	C1—C2	1.480 (3)
Tb1—O2w	2.4042 (17)	C2—C3	1.394 (3)
Tb1—O3w	2.4227 (18)	C2—C7	1.398 (3)
Tb1—O2	2.4276 (16)	C3—C4	1.385 (3)
Tb1—O1	2.4388 (17)	C3—H3A	0.9500
Tb1—O1w	2.4482 (17)	C4—C5	1.386 (3)
O1—C1	1.262 (3)	C4—H4	0.9500
O2—C1	1.280 (3)	C5—C6	1.398 (3)
O3—C5	1.364 (3)	C6—C7	1.383 (3)
O3—H3	0.837 (10)	C6—H6A	0.9500
O4—C8	1.256 (3)	C7—H7	0.9500
O5—C8	1.265 (3)	C8—C9	1.494 (3)
O6—C12	1.370 (3)	C9—C10	1.387 (3)
O6—H6	0.833 (10)	C9—C14	1.395 (4)
O7—C15	1.262 (3)	C10—C11	1.395 (3)
O8—C15	1.262 (3)	C10—H10	0.9500
O8—Tb1ⁱ	2.3276 (16)	C11—C12	1.375 (4)
O9—C19	1.368 (3)	C11—H11A	0.9500
O9—H9	0.841 (10)	C12—C13	1.389 (4)
O1w—H11	0.839 (10)	C13—C14	1.392 (3)
O1w—H12	0.834 (10)	C13—H13	0.9500
O2w—H21	0.838 (10)	C14—H14	0.9500
O2w—H22	0.832 (10)	C15—C16	1.499 (3)
O3w—H31	0.835 (10)	C16—C21	1.395 (3)
O3w—H32	0.840 (10)	C16—C17	1.397 (3)
O4w—H41	0.837 (10)	C17—C18	1.389 (3)
O4w—H42	0.840 (10)	C17—H17	0.9500
O5w—H51	0.861 (10)	C18—C19	1.394 (3)
O5w—H52	0.852 (10)	C18—H18	0.9500
O6w—H61	0.846 (10)	C19—C20	1.394 (3)
O6w—H62	0.841 (10)	C20—C21	1.394 (3)
O7w—H71	0.842 (10)	C20—H20	0.9500
O7w—H72	0.833 (10)	C21—H21A	0.9500

O4—Tb1—O7	147.98 (6)	C4—C3—H3A	119.9
O4—Tb1—O8ⁱ	86.52 (6)	C2—C3—H3A	119.9
O7—Tb1—O8ⁱ	97.15 (6)	C3—C4—C5	119.7 (2)
O4—Tb1—O2w	71.93 (6)	C3—C4—H4	120.2
O7—Tb1—O2w	138.23 (6)	C5—C4—H4	120.2
O8ⁱ—Tb1—O2w	97.25 (6)	O3—C5—C4	122.0 (2)
O4—Tb1—O3w	136.40 (6)	O3—C5—C6	117.2 (2)
O7—Tb1—O3w	74.94 (6)	C4—C5—C6	120.8 (2)
O8ⁱ—Tb1—O3w	77.43 (6)	C7—C6—C5	119.1 (2)
O2w—Tb1—O3w	70.33 (6)	C7—C6—H6A	120.4
O4—Tb1—O2	76.79 (6)	C5—C6—H6A	120.4
O7—Tb1—O2	83.64 (6)	C6—C7—C2	120.5 (2)
O8ⁱ—Tb1—O2	147.37 (6)	C6—C7—H7	119.8
O2w—Tb1—O2	103.72 (6)	C2—C7—H7	119.8
O3w—Tb1—O2	133.16 (6)	O4—C8—O5	122.9 (2)
O4—Tb1—O1	108.71 (6)	O4—C8—C9	117.9 (2)
O7—Tb1—O1	78.16 (6)	O5—C8—C9	119.2 (2)
O8ⁱ—Tb1—O1	158.46 (6)	C10—C9—C14	119.2 (2)
O2w—Tb1—O1	74.23 (6)	C10—C9—C8	120.3 (2)
O3w—Tb1—O1	81.06 (6)	C14—C9—C8	120.4 (2)
O2—Tb1—O1	53.69 (6)	C9—C10—C11	120.4 (2)
O4—Tb1—O1w	78.28 (6)	C9—C10—H10	119.8
O7—Tb1—O1w	73.07 (6)	C11—C10—H10	119.8
O8ⁱ—Tb1—O1w	70.82 (6)	C12—C11—C10	119.7 (2)
O2w—Tb1—O1w	148.59 (6)	C12—C11—H11A	120.2
O3w—Tb1—O1w	130.93 (6)	C10—C11—H11A	120.2
O2—Tb1—O1w	78.37 (6)	O6—C12—C11	116.8 (2)
O1—Tb1—O1w	126.13 (6)	O6—C12—C13	122.2 (2)
C1—O1—Tb1	93.28 (14)	C11—C12—C13	121.0 (2)
C1—O2—Tb1	93.32 (14)	C14—C13—C12	119.1 (2)
C5—O3—H3	107 (2)	C14—C13—H13	120.5
C8—O4—Tb1	150.98 (16)	C12—C13—H13	120.5
C12—O6—H6	114 (2)	C13—C14—C9	120.6 (2)
C15—O7—Tb1	150.17 (16)	C13—C14—H14	119.7
C15—O8—Tb1ⁱ	136.88 (15)	C9—C14—H14	119.7
C19—O9—H9	113 (2)	O8—C15—O7	123.1 (2)
Tb1—O1w—H11	125.7 (19)	O8—C15—C16	117.9 (2)
Tb1—O1w—H12	121.8 (19)	O7—C15—C16	119.0 (2)
H11—O1w—H12	109.2 (16)	C21—C16—C17	119.4 (2)
Tb1—O2w—H21	118 (2)	C21—C16—C15	119.8 (2)
Tb1—O2w—H22	110 (2)	C17—C16—C15	120.8 (2)
H21—O2w—H22	110.7 (16)	C18—C17—C16	120.3 (2)
Tb1—O3w—H31	121 (2)	C18—C17—H17	119.8
Tb1—O3w—H32	114.7 (19)	C16—C17—H17	119.8
H31—O3w—H32	109.5 (16)	C17—C18—C19	119.7 (2)
H41—O4w—H42	108.8 (16)	C17—C18—H18	120.1
H51—O5w—H52	105.4 (15)	C19—C18—H18	120.1
H61—O6w—H62	108.3 (16)	O9—C19—C18	122.6 (2)
H71—O7w—H72	108.9 (16)	O9—C19—C20	116.8 (2)
H81—O8w—H82	109.5 (16)	C18—C19—C20	120.6 (2)
O1—C1—O2	119.7 (2)	C21—C20—C19	119.2 (2)
O1—C1—C2	120.5 (2)	C21—C20—H20	120.4
O2—C1—C2	119.7 (2)	C19—C20—H20	120.4
C3—C2—C7	119.6 (2)	C20—C21—C16	120.7 (2)
C3—C2—C1	120.0 (2)	C20—C21—H21A	119.7
C7—C2—C1	120.2 (2)	C16—C21—H21A	119.7
C4—C3—C2	120.2 (2)

O4—Tb1—O1—C1	−56.96 (14)	C3—C4—C5—C6	3.5 (3)
O7—Tb1—O1—C1	90.56 (14)	O3—C5—C6—C7	176.6 (2)
O8ⁱ—Tb1—O1—C1	169.90 (15)	C4—C5—C6—C7	−3.4 (3)
O2w—Tb1—O1—C1	−121.11 (14)	C5—C6—C7—C2	0.5 (3)
O3w—Tb1—O1—C1	166.92 (14)	C3—C2—C7—C6	2.3 (3)
O2—Tb1—O1—C1	−0.22 (12)	C1—C2—C7—C6	−171.8 (2)
O1w—Tb1—O1—C1	31.99 (16)	Tb1—O4—C8—O5	−108.1 (3)
O4—Tb1—O2—C1	125.77 (14)	Tb1—O4—C8—C9	72.0 (4)
O7—Tb1—O2—C1	−79.74 (13)	O4—C8—C9—C10	−156.2 (2)
O8ⁱ—Tb1—O2—C1	−173.07 (12)	O5—C8—C9—C10	23.8 (3)
O2w—Tb1—O2—C1	58.44 (14)	O4—C8—C9—C14	21.5 (3)
O3w—Tb1—O2—C1	−17.32 (16)	O5—C8—C9—C14	−158.5 (2)
O1—Tb1—O2—C1	0.22 (12)	C14—C9—C10—C11	−1.5 (4)
O1w—Tb1—O2—C1	−153.71 (14)	C8—C9—C10—C11	176.2 (2)
O7—Tb1—O4—C8	66.9 (4)	C9—C10—C11—C12	1.9 (4)
O8ⁱ—Tb1—O4—C8	−31.0 (3)	C10—C11—C12—O6	179.8 (2)
O2w—Tb1—O4—C8	−129.8 (3)	C10—C11—C12—C13	−0.1 (4)
O3w—Tb1—O4—C8	−98.7 (3)	O6—C12—C13—C14	178.0 (2)
O2—Tb1—O4—C8	120.8 (3)	C11—C12—C13—C14	−2.1 (4)
O1—Tb1—O4—C8	164.6 (3)	C12—C13—C14—C9	2.4 (4)
O1w—Tb1—O4—C8	40.1 (3)	C10—C9—C14—C13	−0.7 (4)
O4—Tb1—O7—C15	169.6 (3)	C8—C9—C14—C13	−178.4 (2)
O8ⁱ—Tb1—O7—C15	−95.6 (3)	Tb1ⁱ—O8—C15—O7	14.8 (4)
O2w—Tb1—O7—C15	13.8 (3)	Tb1ⁱ—O8—C15—C16	−163.99 (16)
O3w—Tb1—O7—C15	−20.7 (3)	Tb1—O7—C15—O8	81.1 (4)
O2—Tb1—O7—C15	117.3 (3)	Tb1—O7—C15—C16	−100.2 (3)
O1—Tb1—O7—C15	63.1 (3)	O8—C15—C16—C21	167.8 (2)
O1w—Tb1—O7—C15	−163.0 (3)	O7—C15—C16—C21	−11.1 (3)
Tb1—O1—C1—O2	0.4 (2)	O8—C15—C16—C17	−10.6 (3)
Tb1—O1—C1—C2	−176.78 (18)	O7—C15—C16—C17	170.5 (2)
Tb1—O2—C1—O1	−0.4 (2)	C21—C16—C17—C18	−0.9 (3)
Tb1—O2—C1—C2	176.80 (18)	C15—C16—C17—C18	177.6 (2)
O1—C1—C2—C3	−7.7 (3)	C16—C17—C18—C19	0.0 (3)
O2—C1—C2—C3	175.1 (2)	C17—C18—C19—O9	−179.5 (2)
O1—C1—C2—C7	166.3 (2)	C17—C18—C19—C20	1.2 (4)
O2—C1—C2—C7	−10.8 (3)	O9—C19—C20—C21	179.2 (2)
C7—C2—C3—C4	−2.3 (3)	C18—C19—C20—C21	−1.5 (4)
C1—C2—C3—C4	171.8 (2)	C19—C20—C21—C16	0.5 (3)
C2—C3—C4—C5	−0.6 (4)	C17—C16—C21—C20	0.6 (3)
C3—C4—C5—O3	−176.5 (2)	C15—C16—C21—C20	−177.8 (2)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3···O7wⁱⁱ	0.84 (1)	1.82 (2)	2.612 (3)	158 (3)
O6—H6···O6wⁱⁱⁱ	0.83 (1)	1.87 (1)	2.678 (3)	165 (4)
O9—H9···O4w^iv	0.84 (1)	1.98 (2)	2.763 (3)	156 (3)
O1w—H11···O4w	0.84 (1)	2.04 (1)	2.870 (3)	171 (3)
O1w—H12···O9^v	0.83 (1)	1.96 (1)	2.766 (3)	164 (3)
O2w—H22···O5w	0.83 (1)	1.86 (1)	2.678 (3)	167 (3)
O2w—H21···O5w^vi	0.84 (1)	2.20 (2)	2.952 (3)	150 (3)
O3w—H31···O3ⁱⁱⁱ	0.84 (1)	1.95 (1)	2.777 (3)	171 (3)
O3w—H32···O7ⁱ	0.84 (1)	2.25 (2)	2.916 (2)	137 (3)
O4w—H41···O8w^vii	0.84 (1)	1.94 (1)	2.753 (3)	163 (3)
O4w—H42···O5^viii	0.84 (1)	2.10 (1)	2.927 (3)	169 (3)
O5w—H52···O7w	0.85 (1)	2.01 (2)	2.811 (3)	157 (3)
O5w—H51···O8w^ix	0.86 (1)	1.96 (1)	2.791 (3)	163 (3)
O6w—H61···O2	0.85 (1)	1.90 (1)	2.743 (2)	172 (3)
O6w—H62···O5	0.84 (1)	1.95 (1)	2.785 (2)	171 (3)
O7w—H71···O6w	0.84 (1)	1.90 (1)	2.732 (3)	172 (3)
O7w—H72···O5^x	0.83 (1)	1.89 (1)	2.725 (3)	175 (3)
O8w—H81···O1^xi	0.84 (1)	2.10 (2)	2.818 (3)	144 (3)
O8w—H82···O6	0.84 (1)	1.90 (1)	2.713 (3)	164 (3)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+2, −y+1, −z; (iii) x−1, y, z; (iv) x+1, y+1, z; (v) −x+2, −y+1, −z+1; (vi) −x+1, −y+1, −z; (vii) −x, −y, −z+1; (viii) −x+1, −y, −z+1; (ix) −x, −y, −z; (x) −x+1, −y, −z; (xi) x−1, y−1, z.

Experimental details

Crystal data
Chemical formula	[Tb₂(C₇H₅O₃)₆(H₂O)₆]·10H₂O
M_r	1428.76
Crystal system, space group	Triclinic, P1
Temperature (K)	173
a, b, c (Å)	10.8308 (5), 11.3337 (6), 11.5128 (6)
α, β, γ (°)	90.463 (1), 101.690 (1), 105.249 (1)
V (Å³)	1332.37 (12)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	2.73
Crystal size (mm)	0.47 × 0.30 × 0.19

Data collection
Diffractometer	Bruker SMART area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.360, 0.625
No. of measured, independent and observed [I > 2σ(I)] reflections	12836, 5756, 5391
R_int	0.018
(sin θ/λ)_max (Å⁻¹)	0.639

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.018, 0.059, 1.09
No. of reflections	5756
No. of parameters	409
No. of restraints	27
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.67, −0.64

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2009).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3···O7wⁱ	0.84 (1)	1.82 (2)	2.612 (3)	158 (3)
O6—H6···O6wⁱⁱ	0.83 (1)	1.87 (1)	2.678 (3)	165 (4)
O9—H9···O4wⁱⁱⁱ	0.84 (1)	1.98 (2)	2.763 (3)	156 (3)
O1w—H11···O4w	0.84 (1)	2.04 (1)	2.870 (3)	171 (3)
O1w—H12···O9^iv	0.83 (1)	1.96 (1)	2.766 (3)	164 (3)
O2w—H22···O5w	0.83 (1)	1.86 (1)	2.678 (3)	167 (3)
O2w—H21···O5w^v	0.84 (1)	2.20 (2)	2.952 (3)	150 (3)
O3w—H31···O3ⁱⁱ	0.84 (1)	1.95 (1)	2.777 (3)	171 (3)
O3w—H32···O7^vi	0.84 (1)	2.25 (2)	2.916 (2)	137 (3)
O4w—H41···O8w^vii	0.84 (1)	1.94 (1)	2.753 (3)	163 (3)
O4w—H42···O5^viii	0.84 (1)	2.10 (1)	2.927 (3)	169 (3)
O5w—H52···O7w	0.85 (1)	2.01 (2)	2.811 (3)	157 (3)
O5w—H51···O8w^ix	0.86 (1)	1.96 (1)	2.791 (3)	163 (3)
O6w—H61···O2	0.85 (1)	1.90 (1)	2.743 (2)	172 (3)
O6w—H62···O5	0.84 (1)	1.95 (1)	2.785 (2)	171 (3)
O7w—H71···O6w	0.84 (1)	1.90 (1)	2.732 (3)	172 (3)
O7w—H72···O5^x	0.83 (1)	1.89 (1)	2.725 (3)	175 (3)
O8w—H81···O1^xi	0.84 (1)	2.10 (2)	2.818 (3)	144 (3)
O8w—H82···O6	0.84 (1)	1.90 (1)	2.713 (3)	164 (3)

Symmetry codes: (i) −x+2, −y+1, −z; (ii) x−1, y, z; (iii) x+1, y+1, z; (iv) −x+2, −y+1, −z+1; (v) −x+1, −y+1, −z; (vi) −x+1, −y+1, −z+1; (vii) −x, −y, −z+1; (viii) −x+1, −y, −z+1; (ix) −x, −y, −z; (x) −x+1, −y, −z; (xi) x−1, y−1, z.

Acknowledgements

This work was supported by Sun Yat-Sen University and the University of Malaya.

References

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191. CrossRef CAS Google Scholar
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