catena-Poly[[[diaqua­(3-nitro­benzoato-κ2O,O′)erbium(III)]-di-μ-3-nitro­benzoato-κ4O:O′] 2,2′-diamino-4,4′-bi-1,3-thia­zole]

Liu, B.-X.; Chen, G.-H.; Zhang, L.-J.

doi:10.1107/S1600536807037087

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catena-Poly[[[diaqua(3-nitrobenzoato-κ²O,O′)erbium(III)]-di-μ-3-nitrobenzoato-κ⁴O:O′] 2,2′-diamino-4,4′-bi-1,3-thiazole]

B.-X. Liu, G.-H. Chen and L.-J. Zhang

In the title compound, {[Er(C₇H₄NO₄)₃(H₂O)₂]·C₆H₆N₄S₂}_n, the Er^III ion displays a distorted tetragonal-antiprismatic coordination geometry, formed by five 3-nitrobenzoate anions and two water molecules. Among the three crystallographically independent nitrobenzoate anions, one chelates an Er^III ion and two bridge adjacent Er^III ions to form a one-dimensional polymeric chain extending along the a axis. The uncoordinated diaminobithiazole molecules are centrosymmetric and link with the Er^III complex via hydrogen bonding.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807037087/xu2305sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807037087/xu2305Isup2.hkl Contains datablock I

CCDC reference: 660048

checkCIF report

Key indicators

Single-crystal X-ray study
T = 295 K
Mean (C-C) = 0.008 Å
R factor = 0.032
wR factor = 0.066
Data-to-parameter ratio = 12.5

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal  (x 10000)        100 Deg.
PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 =          4
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       3.28 Ratio
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        N21
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        N31
PLAT323_ALERT_2_C Check Hybridisation of  S41    in Solvent/Ion             ?
PLAT323_ALERT_2_C Check Hybridisation of  S51    in Solvent/Ion             ?
PLAT420_ALERT_2_C D-H Without Acceptor       N52    -   H52B   ...          ?
PLAT432_ALERT_2_C Short Inter X...Y Contact  O13    ..  C41     ..       2.99 Ang.

Alert level G
PLAT794_ALERT_5_G Check Predicted Bond Valency for Er          (3)       3.11

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  10 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   7 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

Comment top

As part of our ongoing investigation on metal complexes with diaminobithiazole (DABT) ligand (Wu et al., 2003; Luo et al., 2004; Liu & Xu, 2004), the title Er^III complex was recently prepared and its X-ray structure is presented here.

The molecular structure of the title compound is shown in Fig. 1. The Er^III has a distorted tetragonal antiprism coordination geometry (Table 1), formed by five 3-nitrobenzoate anions and two water molecules. One 3-nitrobenzoate anion chelates to Er^III ion by the carboxyl group, another four 3-nitrobenzoate anions bridge Er^III ions to form the polymeric complex chain. The C17-carboxyl group makes a dihedral angle of 28.2 (3)° with the benzene ring. The C2-carboxylate group and C37-carboxyl group make different dihedral angles with the benzene rings, 2.4 (4) and 17.5 (6)°, respectively. The average bond length 2.272 (3) Å of Er—O_bridging is shorter than average Er—O_chelating bond length of 2.436 (3) Å.

The DABT molecules located on individual inversion centers display a trans configuration, which agrees with that found in a uncoordinated DABT (Liu et al., 2003). The DABT molecules linked two neighboring complex to form the supra-molecular chains by N—H···O and O—H···N hydrogen bonding (Fig. 1., Table 2). This bridging feature of DABT molecule agrees with that found in (C₆H₈N₄S₂)^2+.2(C₆H₇N₄S₂)^+.4(C₇H₄NO₄)^- reported previously (Liu et al., 2005).

Related literature top

For general background, see: Wu et al. (2003); Luo et al. (2004); Liu & Xu (2004). For related structures, see: Liu et al. (2003, 2005).

Experimental top

An ethanol solution (20 ml) containing diaminobithiazole (DABT) (0.23 g, 1.14 mmol) and ErCl₃^.6H₂O (0.22 g, 0.57 mmol) was mixed with an aqueous solution (10 ml) of 3-nitrobenzoic acid (0.19 g, 1.14 mmol) and NaOH (0.05 g, 1.14 mmol). The mixture was refluxed for 6 h. After cooling to room temperature the solution was filtered. Single crystals of the title compound were obtained from the filtrate after 7 d.

Structure description top

For general background, see: Wu et al. (2003); Luo et al. (2004); Liu & Xu (2004). For related structures, see: Liu et al. (2003, 2005).

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top

Fig. 1. The molecular structure of the title compound with 30% probability displacement ellipsoids (arbitrary spheres for H atoms), dashed lines showing the hydrogen bonding [symmetry codes: (i) -x,1 - y,1 - z; (ii) 1 - x, 1 - y, 1 - z; (iii) -x, 2 - y, 1 - z; (iv) x, 1 + y, z; (v) -2 - x, 1 - y, -z].

catena-Poly[[[diaqua(3-nitrobenzoato-κ²O,O')erbium(III)]-di-µ-3-\ nitrobenzoato-κ⁴O:O'] 2,2'-diamino-4,4'-bi-1,3-thiazole] top

Crystal data top

[Er(C₇H₄NO₄)₃(H₂O)₂]·C₆H₆N₄S₂	Z = 2
M_r = 899.90	F(000) = 890
Triclinic, P1	D_x = 1.814 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.6739 (7) Å	Cell parameters from 5670 reflections
b = 12.993 (1) Å	θ = 2.0–25.0°
c = 14.5927 (11) Å	µ = 2.75 mm⁻¹
α = 68.148 (1)°	T = 295 K
β = 86.352 (1)°	Prism, red
γ = 75.553 (1)°	0.20 × 0.17 × 0.14 mm
V = 1647.7 (2) Å³

Data collection top

Rigaku R-AXIS RAPID IP diffractometer	5731 independent reflections
Radiation source: fine-focus sealed tube	5127 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.022
Detector resolution: 10.0 pixels mm^-1	θ_max = 25.0°, θ_min = 2.1°
ω scans	h = −9→11
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −12→15
T_min = 0.560, T_max = 0.680	l = −16→17
8623 measured reflections

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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.066	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0253P)² + 0.8606P] where P = (F_o² + 2F_c²)/3
5731 reflections	(Δ/σ)_max = 0.001
460 parameters	Δρ_max = 0.56 e Å⁻³
0 restraints	Δρ_min = −0.73 e Å⁻³

Crystal data top

[Er(C₇H₄NO₄)₃(H₂O)₂]·C₆H₆N₄S₂	γ = 75.553 (1)°
M_r = 899.90	V = 1647.7 (2) Å³
Triclinic, P1	Z = 2
a = 9.6739 (7) Å	Mo Kα radiation
b = 12.993 (1) Å	µ = 2.75 mm⁻¹
c = 14.5927 (11) Å	T = 295 K
α = 68.148 (1)°	0.20 × 0.17 × 0.14 mm
β = 86.352 (1)°

Data collection top

Rigaku R-AXIS RAPID IP diffractometer	5731 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	5127 reflections with I > 2σ(I)
T_min = 0.560, T_max = 0.680	R_int = 0.022
8623 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.032	0 restraints
wR(F²) = 0.066	H-atom parameters constrained
S = 1.04	Δρ_max = 0.56 e Å⁻³
5731 reflections	Δρ_min = −0.73 e Å⁻³
460 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
Er	0.23836 (2)	0.534282 (16)	0.488335 (14)	0.02794 (7)
O1	0.0653 (3)	0.7073 (2)	0.4698 (2)	0.0404 (8)
H1A	−0.0140	0.6984	0.4654	0.048*
H1B	0.0630	0.7445	0.5034	0.048*
O2	0.3274 (3)	0.6254 (3)	0.5816 (2)	0.0411 (8)
H2A	0.4053	0.5942	0.6099	0.049*
H2B	0.3058	0.6920	0.5776	0.049*
O11	0.3646 (3)	0.4181 (3)	0.3984 (2)	0.0411 (8)
O12	0.2065 (3)	0.3474 (2)	0.5022 (2)	0.0378 (7)
O13	0.3152 (4)	−0.0827 (3)	0.5920 (3)	0.0612 (10)
O14	0.3511 (4)	−0.1456 (3)	0.4731 (3)	0.0708 (12)
O21	0.0899 (3)	0.5813 (3)	0.3549 (2)	0.0439 (8)
O22	−0.1017 (3)	0.5123 (3)	0.3786 (2)	0.0446 (8)
O23	−0.4305 (5)	0.6104 (5)	0.1072 (4)	0.1089 (19)
O24	−0.4168 (5)	0.7462 (4)	−0.0301 (3)	0.1030 (17)
O31	0.3488 (3)	0.6566 (3)	0.3733 (2)	0.0420 (8)
O32	0.5808 (3)	0.5949 (3)	0.4063 (2)	0.0453 (8)
O33	0.7828 (6)	1.0268 (5)	0.1239 (4)	0.124 (2)
O34	0.8555 (5)	0.8901 (5)	0.2628 (4)	0.0907 (15)
N11	0.3339 (4)	−0.0681 (4)	0.5054 (4)	0.0508 (11)
N21	−0.3713 (6)	0.6810 (5)	0.0532 (4)	0.0677 (15)
N31	0.7672 (6)	0.9441 (5)	0.1964 (4)	0.0699 (14)
N41	0.0331 (4)	0.8453 (3)	0.5768 (3)	0.0332 (8)
N42	0.0566 (5)	0.6783 (3)	0.7180 (3)	0.0520 (11)
H42A	0.0793	0.6283	0.6901	0.062*
H42B	0.0619	0.6540	0.7798	0.062*
N51	−0.8833 (4)	0.5964 (3)	−0.0659 (3)	0.0472 (10)
N52	−0.6912 (5)	0.6844 (4)	−0.0938 (4)	0.0840 (17)
H52A	−0.6039	0.6718	−0.0733	0.101*
H52B	−0.7197	0.7411	−0.1494	0.101*
S41	−0.00548 (15)	0.88246 (11)	0.73874 (9)	0.0470 (3)
S51	−0.70468 (15)	0.51627 (13)	0.08145 (11)	0.0623 (4)
C11	0.3284 (5)	0.2406 (4)	0.4055 (3)	0.0366 (11)
C12	0.3083 (4)	0.1363 (4)	0.4694 (4)	0.0368 (11)
H12	0.2738	0.1269	0.5322	0.044*
C13	0.3416 (5)	0.0458 (4)	0.4361 (4)	0.0421 (12)
C14	0.3832 (6)	0.0586 (5)	0.3419 (4)	0.0569 (15)
H14	0.3995	−0.0025	0.3207	0.068*
C15	0.4004 (6)	0.1631 (5)	0.2796 (4)	0.0625 (16)
H15	0.4283	0.1737	0.2152	0.075*
C16	0.3765 (5)	0.2529 (4)	0.3121 (4)	0.0468 (12)
H16	0.3931	0.3225	0.2704	0.056*
C17	0.2972 (5)	0.3413 (4)	0.4373 (3)	0.0359 (11)
C21	−0.0676 (5)	0.6362 (4)	0.2196 (3)	0.0325 (10)
C22	−0.1923 (5)	0.6271 (4)	0.1846 (3)	0.0378 (11)
H22	−0.2463	0.5795	0.2261	0.045*
C23	−0.2346 (6)	0.6900 (4)	0.0871 (4)	0.0494 (13)
C24	−0.1618 (7)	0.7615 (5)	0.0232 (4)	0.0625 (16)
H24	−0.1947	0.8034	−0.0418	0.075*
C25	−0.0383 (7)	0.7705 (5)	0.0570 (4)	0.0637 (16)
H25	0.0150	0.8177	0.0141	0.076*
C26	0.0088 (6)	0.7088 (4)	0.1561 (4)	0.0506 (13)
H26	0.0916	0.7169	0.1788	0.061*
C27	−0.0222 (4)	0.5716 (4)	0.3263 (3)	0.0309 (10)
C31	0.4937 (5)	0.7748 (4)	0.2790 (3)	0.0324 (10)
C32	0.6194 (5)	0.8086 (4)	0.2749 (3)	0.0384 (11)
H32	0.6927	0.7653	0.3219	0.046*
C33	0.6337 (6)	0.9073 (4)	0.2003 (4)	0.0456 (12)
C34	0.5288 (7)	0.9735 (5)	0.1300 (4)	0.0635 (16)
H34	0.5415	1.0401	0.0802	0.076*
C35	0.4040 (7)	0.9397 (5)	0.1343 (4)	0.0663 (17)
H35	0.3314	0.9835	0.0869	0.080*
C36	0.3857 (5)	0.8404 (4)	0.2091 (4)	0.0502 (13)
H36	0.3008	0.8182	0.2121	0.060*
C37	0.4740 (5)	0.6664 (3)	0.3589 (3)	0.0297 (9)
C41	0.0016 (4)	0.9632 (3)	0.5521 (3)	0.0314 (10)
C42	−0.0232 (5)	0.9975 (4)	0.6293 (3)	0.0407 (11)
H42	−0.0468	1.0734	0.6240	0.049*
C43	0.0330 (5)	0.7925 (4)	0.6719 (3)	0.0365 (11)
C51	−0.9334 (5)	0.5121 (4)	0.0086 (3)	0.0415 (11)
C52	−0.8513 (5)	0.4608 (5)	0.0911 (4)	0.0544 (14)
H52	−0.8710	0.4025	0.1468	0.065*
C53	−0.7648 (6)	0.6076 (4)	−0.0381 (4)	0.0516 (13)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Er	0.02554 (11)	0.02397 (11)	0.03386 (12)	−0.00788 (8)	−0.00287 (8)	−0.00838 (8)
O1	0.0322 (17)	0.0376 (18)	0.056 (2)	−0.0026 (14)	−0.0047 (15)	−0.0251 (16)
O2	0.0345 (17)	0.0352 (18)	0.058 (2)	−0.0059 (14)	−0.0066 (15)	−0.0228 (16)
O11	0.0404 (18)	0.0341 (18)	0.054 (2)	−0.0135 (15)	0.0042 (15)	−0.0201 (16)
O12	0.0384 (18)	0.0296 (17)	0.0514 (19)	−0.0152 (14)	0.0035 (15)	−0.0176 (15)
O13	0.051 (2)	0.043 (2)	0.080 (3)	−0.0158 (18)	−0.005 (2)	−0.008 (2)
O14	0.063 (2)	0.034 (2)	0.124 (4)	−0.0105 (18)	−0.001 (2)	−0.039 (2)
O21	0.0432 (19)	0.042 (2)	0.0489 (19)	−0.0117 (15)	−0.0143 (16)	−0.0164 (16)
O22	0.0453 (19)	0.049 (2)	0.0373 (18)	−0.0163 (16)	0.0048 (15)	−0.0105 (16)
O23	0.084 (4)	0.136 (5)	0.108 (4)	−0.049 (3)	−0.039 (3)	−0.025 (4)
O24	0.115 (4)	0.098 (4)	0.077 (3)	0.009 (3)	−0.060 (3)	−0.024 (3)
O31	0.0346 (18)	0.0390 (19)	0.0487 (19)	−0.0168 (15)	0.0032 (15)	−0.0073 (16)
O32	0.0420 (19)	0.0265 (17)	0.056 (2)	−0.0037 (15)	−0.0204 (16)	−0.0017 (15)
O33	0.148 (5)	0.100 (4)	0.128 (4)	−0.095 (4)	0.034 (4)	−0.011 (4)
O34	0.085 (3)	0.102 (4)	0.113 (4)	−0.063 (3)	0.011 (3)	−0.047 (3)
N11	0.030 (2)	0.037 (3)	0.084 (4)	−0.0081 (19)	−0.007 (2)	−0.020 (3)
N21	0.069 (4)	0.068 (4)	0.068 (4)	0.005 (3)	−0.032 (3)	−0.035 (3)
N31	0.087 (4)	0.063 (4)	0.080 (4)	−0.051 (3)	0.023 (3)	−0.032 (3)
N41	0.036 (2)	0.031 (2)	0.033 (2)	−0.0119 (16)	0.0000 (16)	−0.0103 (17)
N42	0.081 (3)	0.031 (2)	0.037 (2)	−0.012 (2)	0.004 (2)	−0.0067 (19)
N51	0.048 (3)	0.043 (2)	0.047 (2)	−0.015 (2)	−0.006 (2)	−0.009 (2)
N52	0.062 (3)	0.083 (4)	0.084 (4)	−0.035 (3)	−0.013 (3)	0.009 (3)
S41	0.0646 (8)	0.0419 (7)	0.0350 (6)	−0.0115 (6)	0.0013 (6)	−0.0157 (6)
S51	0.0514 (8)	0.0658 (10)	0.0603 (9)	−0.0205 (7)	−0.0158 (7)	−0.0058 (7)
C11	0.035 (3)	0.026 (2)	0.046 (3)	−0.0019 (19)	−0.011 (2)	−0.012 (2)
C12	0.030 (2)	0.031 (3)	0.052 (3)	−0.0052 (19)	−0.004 (2)	−0.019 (2)
C13	0.034 (3)	0.028 (3)	0.062 (3)	−0.006 (2)	−0.010 (2)	−0.013 (2)
C14	0.061 (4)	0.048 (3)	0.073 (4)	−0.007 (3)	−0.011 (3)	−0.037 (3)
C15	0.086 (4)	0.056 (4)	0.049 (3)	−0.010 (3)	−0.005 (3)	−0.026 (3)
C16	0.058 (3)	0.034 (3)	0.045 (3)	−0.009 (2)	−0.013 (2)	−0.010 (2)
C17	0.031 (2)	0.029 (2)	0.047 (3)	−0.004 (2)	−0.011 (2)	−0.013 (2)
C21	0.037 (2)	0.028 (2)	0.033 (2)	−0.0051 (19)	0.0001 (19)	−0.013 (2)
C22	0.039 (3)	0.035 (3)	0.039 (3)	−0.005 (2)	−0.004 (2)	−0.016 (2)
C23	0.057 (3)	0.043 (3)	0.045 (3)	−0.001 (3)	−0.018 (3)	−0.016 (3)
C24	0.096 (5)	0.046 (3)	0.035 (3)	−0.007 (3)	−0.012 (3)	−0.008 (3)
C25	0.089 (5)	0.048 (3)	0.046 (3)	−0.025 (3)	0.015 (3)	−0.005 (3)
C26	0.057 (3)	0.043 (3)	0.055 (3)	−0.020 (3)	0.003 (3)	−0.017 (3)
C27	0.029 (2)	0.027 (2)	0.036 (2)	−0.0031 (19)	−0.001 (2)	−0.014 (2)
C31	0.036 (2)	0.025 (2)	0.034 (2)	−0.0071 (19)	−0.0001 (19)	−0.0084 (19)
C32	0.043 (3)	0.030 (3)	0.044 (3)	−0.010 (2)	0.003 (2)	−0.015 (2)
C33	0.061 (3)	0.039 (3)	0.048 (3)	−0.027 (3)	0.016 (3)	−0.020 (2)
C34	0.099 (5)	0.038 (3)	0.047 (3)	−0.027 (3)	0.011 (3)	−0.002 (3)
C35	0.080 (4)	0.049 (3)	0.051 (3)	−0.012 (3)	−0.019 (3)	0.004 (3)
C36	0.046 (3)	0.045 (3)	0.049 (3)	−0.010 (2)	−0.008 (2)	−0.004 (3)
C37	0.035 (3)	0.026 (2)	0.033 (2)	−0.0092 (19)	−0.001 (2)	−0.0144 (19)
C41	0.029 (2)	0.028 (2)	0.038 (2)	−0.0084 (19)	0.0013 (19)	−0.012 (2)
C42	0.050 (3)	0.030 (3)	0.041 (3)	−0.009 (2)	−0.004 (2)	−0.012 (2)
C43	0.040 (3)	0.034 (3)	0.040 (3)	−0.012 (2)	0.001 (2)	−0.017 (2)
C51	0.040 (3)	0.039 (3)	0.041 (3)	−0.008 (2)	−0.002 (2)	−0.009 (2)
C52	0.050 (3)	0.054 (3)	0.052 (3)	−0.018 (3)	−0.004 (3)	−0.008 (3)
C53	0.048 (3)	0.045 (3)	0.054 (3)	−0.014 (3)	−0.003 (3)	−0.008 (3)

Geometric parameters (Å, º) top

Er—O1	2.378 (3)	S51—C52	1.721 (5)
Er—O2	2.419 (3)	S51—C53	1.742 (5)
Er—O11	2.417 (3)	C11—C16	1.376 (6)
Er—O12	2.455 (3)	C11—C12	1.382 (6)
Er—O21	2.293 (3)	C11—C17	1.502 (6)
Er—O22ⁱ	2.254 (3)	C12—C13	1.392 (6)
Er—O31	2.262 (3)	C12—H12	0.9300
Er—O32ⁱⁱ	2.280 (3)	C13—C14	1.368 (7)
Er—C17	2.791 (4)	C14—C15	1.369 (8)
O1—H1A	0.8137	C14—H14	0.9300
O1—H1B	0.8020	C15—C16	1.378 (7)
O2—H2A	0.8155	C15—H15	0.9300
O2—H2B	0.8188	C16—H16	0.9300
O11—C17	1.265 (5)	C21—C26	1.379 (6)
O12—C17	1.261 (5)	C21—C22	1.387 (6)
O13—N11	1.214 (5)	C21—C27	1.500 (6)
O14—N11	1.235 (5)	C22—C23	1.379 (6)
O21—C27	1.238 (5)	C22—H22	0.9300
O22—C27	1.245 (5)	C23—C24	1.351 (8)
O22—Erⁱ	2.254 (3)	C24—C25	1.368 (8)
O23—N21	1.207 (7)	C24—H24	0.9300
O24—N21	1.227 (6)	C25—C26	1.407 (7)
O31—C37	1.246 (5)	C25—H25	0.9300
O32—C37	1.242 (5)	C26—H26	0.9300
O32—Erⁱⁱ	2.280 (3)	C31—C36	1.379 (6)
O33—N31	1.229 (6)	C31—C32	1.383 (6)
O34—N31	1.209 (6)	C31—C37	1.504 (6)
N11—C13	1.467 (6)	C32—C33	1.371 (6)
N21—C23	1.487 (7)	C32—H32	0.9300
N31—C33	1.476 (7)	C33—C34	1.364 (7)
N41—C43	1.299 (5)	C34—C35	1.375 (8)
N41—C41	1.392 (5)	C34—H34	0.9300
N42—C43	1.347 (5)	C35—C36	1.387 (7)
N42—H42A	0.8667	C35—H35	0.9300
N42—H42B	0.8371	C36—H36	0.9300
N51—C53	1.299 (6)	C41—C42	1.346 (6)
N51—C51	1.388 (6)	C41—C41ⁱⁱⁱ	1.461 (8)
N52—C53	1.357 (7)	C42—H42	0.9300
N52—H52A	0.8698	C51—C52	1.336 (6)
N52—H52B	0.8715	C51—C51^iv	1.457 (9)
S41—C42	1.716 (5)	C52—H52	0.9300
S41—C43	1.744 (4)

O22ⁱ—Er—O31	152.41 (12)	C13—C14—C15	118.6 (5)
O22ⁱ—Er—O32ⁱⁱ	84.35 (12)	C13—C14—H14	120.7
O31—Er—O32ⁱⁱ	104.12 (11)	C15—C14—H14	120.7
O22ⁱ—Er—O21	105.35 (11)	C14—C15—C16	120.2 (5)
O31—Er—O21	81.29 (11)	C14—C15—H15	119.9
O32ⁱⁱ—Er—O21	148.41 (11)	C16—C15—H15	119.9
O22ⁱ—Er—O1	75.53 (11)	C11—C16—C15	120.8 (5)
O31—Er—O1	81.78 (11)	C11—C16—H16	119.6
O32ⁱⁱ—Er—O1	140.33 (11)	C15—C16—H16	119.6
O21—Er—O1	70.92 (10)	O12—C17—O11	121.3 (4)
O22ⁱ—Er—O11	129.54 (11)	O12—C17—C11	120.1 (4)
O31—Er—O11	77.98 (11)	O11—C17—C11	118.6 (4)
O32ⁱⁱ—Er—O11	75.16 (11)	O12—C17—Er	61.6 (2)
O21—Er—O11	75.68 (11)	O11—C17—Er	59.8 (2)
O1—Er—O11	143.06 (10)	C11—C17—Er	177.6 (3)
O22ⁱ—Er—O2	81.49 (11)	C26—C21—C22	118.9 (4)
O31—Er—O2	76.92 (11)	C26—C21—C27	121.4 (4)
O32ⁱⁱ—Er—O2	70.61 (10)	C22—C21—C27	119.6 (4)
O21—Er—O2	139.80 (11)	C23—C22—C21	118.7 (5)
O1—Er—O2	72.82 (10)	C23—C22—H22	120.6
O11—Er—O2	130.44 (10)	C21—C22—H22	120.6
O22ⁱ—Er—O12	76.80 (11)	C24—C23—C22	123.6 (5)
O31—Er—O12	130.58 (11)	C24—C23—N21	119.2 (5)
O32ⁱⁱ—Er—O12	75.58 (10)	C22—C23—N21	117.1 (5)
O21—Er—O12	77.55 (10)	C23—C24—C25	118.0 (5)
O1—Er—O12	130.06 (10)	C23—C24—H24	121.0
O11—Er—O12	53.73 (10)	C25—C24—H24	121.0
O2—Er—O12	141.23 (10)	C24—C25—C26	120.5 (5)
O22ⁱ—Er—C17	103.32 (13)	C24—C25—H25	119.7
O31—Er—C17	104.25 (13)	C26—C25—H25	119.7
O32ⁱⁱ—Er—C17	74.21 (12)	C21—C26—C25	120.2 (5)
O21—Er—C17	74.30 (11)	C21—C26—H26	119.9
O1—Er—C17	143.33 (11)	C25—C26—H26	119.9
O11—Er—C17	26.90 (12)	O21—C27—O22	125.5 (4)
O2—Er—C17	143.84 (11)	O21—C27—C21	117.9 (4)
O12—Er—C17	26.84 (11)	O22—C27—C21	116.6 (4)
Er—O1—H1A	109.2	C36—C31—C32	119.9 (4)
Er—O1—H1B	124.7	C36—C31—C37	119.6 (4)
H1A—O1—H1B	109.5	C32—C31—C37	120.5 (4)
Er—O2—H2A	118.2	C33—C32—C31	118.7 (4)
Er—O2—H2B	130.3	C33—C32—H32	120.7
H2A—O2—H2B	108.8	C31—C32—H32	120.7
C17—O11—Er	93.3 (3)	C34—C33—C32	122.6 (5)
C17—O12—Er	91.6 (3)	C34—C33—N31	118.7 (5)
C27—O21—Er	145.7 (3)	C32—C33—N31	118.7 (5)
C27—O22—Erⁱ	150.7 (3)	C33—C34—C35	118.6 (5)
C37—O31—Er	135.7 (3)	C33—C34—H34	120.7
C37—O32—Erⁱⁱ	172.3 (3)	C35—C34—H34	120.7
O13—N11—O14	123.1 (5)	C34—C35—C36	120.3 (5)
O13—N11—C13	118.8 (4)	C34—C35—H35	119.8
O14—N11—C13	118.0 (5)	C36—C35—H35	119.8
O23—N21—O24	123.5 (6)	C31—C36—C35	119.9 (5)
O23—N21—C23	119.4 (5)	C31—C36—H36	120.0
O24—N21—C23	117.1 (6)	C35—C36—H36	120.0
O34—N31—O33	124.0 (6)	O32—C37—O31	124.9 (4)
O34—N31—C33	118.6 (5)	O32—C37—C31	118.8 (4)
O33—N31—C33	117.4 (6)	O31—C37—C31	116.3 (4)
C43—N41—C41	110.9 (4)	C42—C41—N41	114.9 (4)
C43—N42—H42A	126.1	C42—C41—C41ⁱⁱⁱ	126.5 (5)
C43—N42—H42B	115.7	N41—C41—C41ⁱⁱⁱ	118.6 (5)
H42A—N42—H42B	117.5	C41—C42—S41	111.0 (3)
C53—N51—C51	110.9 (4)	C41—C42—H42	124.5
C53—N52—H52A	115.5	S41—C42—H42	124.5
C53—N52—H52B	127.2	N41—C43—N42	124.7 (4)
H52A—N52—H52B	117.2	N41—C43—S41	114.4 (3)
C42—S41—C43	88.8 (2)	N42—C43—S41	120.9 (3)
C52—S51—C53	88.2 (2)	C52—C51—N51	114.7 (4)
C16—C11—C12	120.1 (4)	C52—C51—C51^iv	126.3 (6)
C16—C11—C17	119.6 (4)	N51—C51—C51^iv	119.0 (5)
C12—C11—C17	120.3 (4)	C51—C52—S51	111.5 (4)
C11—C12—C13	117.5 (4)	C51—C52—H52	124.2
C11—C12—H12	121.3	S51—C52—H52	124.2
C13—C12—H12	121.3	N51—C53—N52	124.9 (5)
C14—C13—C12	122.7 (5)	N51—C53—S51	114.6 (4)
C14—C13—N11	118.8 (5)	N52—C53—S51	120.4 (4)
C12—C13—N11	118.5 (5)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O12ⁱ	0.81	2.07	2.857 (4)	163
O1—H1B···N41	0.80	1.94	2.737 (5)	173
O2—H2A···O11ⁱⁱ	0.82	2.19	2.903 (4)	146
O2—H2B···O14^v	0.82	2.23	2.864 (5)	135
N42—H42A···O22ⁱ	0.87	2.35	3.208 (6)	170
N42—H42B···N51^vi	0.84	2.15	2.973 (6)	169
N52—H52A···O24	0.87	2.47	3.239 (7)	148

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (v) x, y+1, z; (vi) x+1, y, z+1.

Experimental details

Crystal data
Chemical formula	[Er(C₇H₄NO₄)₃(H₂O)₂]·C₆H₆N₄S₂
M_r	899.90
Crystal system, space group	Triclinic, P1
Temperature (K)	295
a, b, c (Å)	9.6739 (7), 12.993 (1), 14.5927 (11)
α, β, γ (°)	68.148 (1), 86.352 (1), 75.553 (1)
V (Å³)	1647.7 (2)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.75
Crystal size (mm)	0.20 × 0.17 × 0.14

Data collection
Diffractometer	Rigaku R-AXIS RAPID IP
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.560, 0.680
No. of measured, independent and observed [I > 2σ(I)] reflections	8623, 5731, 5127
R_int	0.022
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.032, 0.066, 1.04
No. of reflections	5731
No. of parameters	460
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.56, −0.73

Computer programs: PROCESS-AUTO (Rigaku, 1998), PROCESS-AUTO, CrystalStructure (Rigaku/MSC, 2002), SIR92 (Altomare et al., 1993), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

Selected bond lengths (Å) top

Er—O1	2.378 (3)	Er—O21	2.293 (3)
Er—O2	2.419 (3)	Er—O22ⁱ	2.254 (3)
Er—O11	2.417 (3)	Er—O31	2.262 (3)
Er—O12	2.455 (3)	Er—O32ⁱⁱ	2.280 (3)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O12ⁱ	0.81	2.07	2.857 (4)	163
O1—H1B···N41	0.80	1.94	2.737 (5)	173
O2—H2A···O11ⁱⁱ	0.82	2.19	2.903 (4)	146
O2—H2B···O14ⁱⁱⁱ	0.82	2.23	2.864 (5)	135
N42—H42A···O22ⁱ	0.87	2.35	3.208 (6)	170
N42—H42B···N51^iv	0.84	2.15	2.973 (6)	169
N52—H52A···O24	0.87	2.47	3.239 (7)	148

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

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