Poly[[tetra­kis­(μ₂-pyrazine N,N′-dioxide-κ²O:O′)dysprosium(III)] tris­(perchlorate)]

The title three-dimensional coordination network, {[Dy(C₄H₄N₂O₂)₄](ClO₄)₃}_n, is isostructural of other lanthanides. The Dy⁺³ cation lies on a fourfold roto-inversion axis. It is coordinated in a distorted square-anti­prismatic fashion by eight O atoms from bridging pyrazine N,N′-dioxide ligands. There are two unique pyrazine N,N′-dioxide ligands. One ring is located around an inversion center, and there is a a twofold rotation axis at the center of the other ring. There are also two unique perchlorate anions. One is centered on a twofold rotation axis and the other on a fourfold roto-inversion axis. The perchlorate anions are located in channels that run perpendicular to (001) and (110) and inter­act with the coordination network through C—H...O hydrogen bonds.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.033
• wR factor = 0.096
• Data-to-parameter ratio = 16.4

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT430_ALERT_2_A Short Inter D...A Contact  O3     ..  O3      ..       2.34 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT430_ALERT_2_A Short Inter D...A Contact  O3     ..  O3      ..       2.36 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT430_ALERT_2_A Short Inter D...A Contact  O3     ..  O3      ..       2.36 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT430_ALERT_2_A Short Inter D...A Contact  O4     ..  O4      ..       2.21 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT430_ALERT_2_A Short Inter D...A Contact  O4     ..  O5      ..       2.29 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT430_ALERT_2_A Short Inter D...A Contact  O5     ..  O5      ..       2.11 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.95
PLAT430_ALERT_2_B Short Inter D...A Contact  O1     ..  O2      ..       2.78 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT430_ALERT_2_B Short Inter D...A Contact  O1     ..  O2      ..       2.82 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT430_ALERT_2_B Short Inter D...A Contact  O2     ..  O2      ..       2.81 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT430_ALERT_2_B Short Inter D...A Contact  N1     ..  N1      ..       2.73 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT430_ALERT_2_B Short Inter D...A Contact  N2     ..  N2      ..       2.74 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT971_ALERT_2_B Large Calcd. Non-Metal Positive Residual Density       2.83 eA-3

Alert level C
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600         58
PLAT971_ALERT_2_C Large Calcd. Non-Metal Positive Residual Density       1.51 eA-3
PLAT973_ALERT_2_C Large Calcd. Positive Residual Density on    Dy1       1.38 eA-3
PLAT041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ          ?
PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.25 Ratio
PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L=  0.600         30
PLAT952_ALERT_1_C Reported and Calculated Lmax Values Differ by ..          7

Alert level G
REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values
           From the CIF: _diffrn_reflns_theta_max           30.49
           From the CIF: _reflns_number_total               1800
           From the CIF: _diffrn_reflns_limit_ max hkl   19.   21.   25.
           From the CIF: _diffrn_reflns_limit_ min hkl  -21.   -3.  -20.
           TEST1: Expected hkl limits for theta max
           Calculated maximum hkl   21.   21.   32.
           Calculated minimum hkl  -21.  -21.  -32.
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large.      37.18
PLAT432_ALERT_2_G Short Inter X...Y Contact  Cl1    ..  O3      ..       1.44 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  Cl1    ..  O3      ..       1.44 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  Cl1    ..  O3      ..       1.44 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  Cl2    ..  O4      ..       1.36 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  Cl2    ..  O5      ..       1.38 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  O1     ..  C2      ..       2.32 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  O1     ..  C3      ..       2.93 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  O2     ..  C4      ..       2.29 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  O2     ..  C2      ..       2.97 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  O3     ..  C1      ..       2.90 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  O4     ..  C4      ..       2.91 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  O5     ..  C4      ..       2.90 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  N1     ..  C2      ..       1.36 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  N1     ..  C1      ..       2.36 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  N2     ..  C4      ..       1.36 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  N2     ..  C3      ..       2.37 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  C1     ..  C2      ..       2.35 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  C1     ..  C1      ..       2.71 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  C2     ..  C2      ..       2.72 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  C3     ..  C4      ..       2.34 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  C3     ..  C3      ..       2.71 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT432_ALERT_2_G Short Inter X...Y Contact  C4     ..  C4      ..       2.70 Ang.

Author Response: All of these errors seem to be incorrect. The program does not seem to be recognizing symmetry generated atoms that are part of the same molecule or ion. For example, the O3-O3 distance of 2.34 ang is between O3 bonded to Cl1 and a symmetry generated O3 also bonded to Cl1. The distance is consistent with O-O distances in perchlorate anions. Also, the Cl1-O3 distance of 1.44 ang. is consistent with Cl-O distances in perchlorate anions.

PLAT804_ALERT_5_G ARU-Pack Problem in PLATON Analysis ............          1 Times

   6 ALERT level A = In general: serious problem
   7 ALERT level B = Potentially serious problem
   8 ALERT level C = Check and explain
  25 ALERT level G = General alerts; check

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

---

S1. Comment

The description of the structure of the title compound is part of a series of consecutive papers on three-dimensional coordination networks of the type {[Ln(C₄H₄N₂O₂)₄](ClO₄)₃}_n, with Ln = Nd (Quinn-Elmore et al. 2010), Dy (this publication), Ho (Buchner et al. 2010a) and Er (Buchner et al. 2010b), respectively. All four compounds are also isostructural to the previously reported La, Ce, Pr, Sm, Eu, Gd, Tb and Y coordination networks (Sun et al. 2004). The background to this study is given in ther first article of this series by Quinn-Elmore et al. (2010).

Related literature

For the isostructural La, Ce, Pr, Sm, Eu, Gd, Tb and Y coordination networks see: Sun et al. (2004). For the isostructural Nd, Ho and Er coordination networks see: Quinn-Elmore et al. (2010); Buchner et al. (2010a,b), respectively. Detailed background to this study is given in the first article of this series by Quinn-Elmore et al. (2010).

S2. Experimental

Pyrazine N,N'-dioxide (0.025 g, 0.223 mmol) was dissolved in deionized water (1.5 ml) and methanol (1.5 ml). An aqueous solution of Dy(ClO₄)₃ (0.320 ml of a 0.0868 M solution, 0.028 mmol) was diluted with methanol (0.680 ml) and CH₂Cl₂ (2.5 ml). The pyrazine N,N'-dioxide solution was layered over the Dy(ClO₄)₃ solution, and the two solutions were allowed to slowly mix. Colorless block-like crystals formed upon the slow evaporation of the resultant solution.

S3. Refinement

All H atoms were positioned geometrically and refined using a riding model with C—H = 0.95Å and with U_iso(H) = 1.2 times U_eq(C).

Computing details

Data collection: SMART (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus (Bruker, 2007); 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: X-SEED (Barbour, 2001).

Figures

Fig. 1. The coordination environment of the Dy^+3 cation in title compound with atom labels and 50% probability displacement ellipsoids. Hydrogen atoms have been omitted for clarity. Symmetry codes: (i) y + 1/4, x - 1/4, -z + 3/4; (ii) -y + 3/4, -x + 3/4, -z + 3/4; (iii) -x + 1, -y + 1/2, z; (iv) -y + 3/4, x - 1/4, -z + 1/4; (v) y + 1/4, -x + 3/4, -z + 1/4; (vi) y + 3/4, x - 3/4, -z + 1/4; (vii) -x + 3/2, -y + 1/2, -z + 1/2; (viii) x, -y + 1, -z + 1/2.

Poly[[tetrakis(µ₂-pyrazine N,N'-dioxide-κ²O:O')dysprosium(III)] tris(perchlorate)]

Crystal data

[Dy(C4H4N2O2)4](ClO4)3	Dx = 2.290 Mg m^−3
Mr = 909.22	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/acd	Cell parameters from 4338 reflections
Hall symbol: -I 4bd 2c	θ = 2.7–30.5°
a = 15.2553 (4) Å	µ = 3.25 mm^−1
c = 22.6667 (12) Å	T = 100 K
V = 5275.1 (3) Å^3	Block, colourless
Z = 8	0.34 × 0.27 × 0.20 mm
F(000) = 3560

Data collection

Bruker SMART APEX CCD diffractometer	1800 independent reflections
Radiation source: fine-focus sealed tube	1493 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.018
ω scans	θmax = 30.5°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −21→19
Tmin = 0.374, Tmax = 0.532	k = −3→21
8476 measured reflections	l = −20→25

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)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.096	H-atom parameters constrained
S = 0.99	w = 1/[σ^2(Fo^2) + (0.0554P)^2 + 37.1849P] where P = (Fo^2 + 2Fc^2)/3
1800 reflections	(Δ/σ)max < 0.001
110 parameters	Δρmax = 2.68 e Å^−3
0 restraints	Δρmin = −1.48 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
Dy1	0.5000	0.2500	0.3750	0.00560 (12)
Cl1	0.5000	0.2500	0.1250	0.0113 (4)
Cl2	0.72654 (6)	−0.02346 (6)	0.1250	0.0281 (3)
O1	0.59121 (12)	0.21876 (14)	0.29510 (10)	0.0155 (4)
O2	0.53217 (14)	0.39451 (12)	0.34383 (10)	0.0153 (4)
O3	0.57642 (16)	0.24419 (16)	0.16207 (12)	0.0251 (6)
O4	0.6466 (4)	−0.0162 (4)	0.1506 (4)	0.137 (3)
O5	0.7912 (4)	−0.0056 (4)	0.1658 (4)	0.129 (3)
N1	0.66943 (16)	0.23424 (16)	0.27415 (13)	0.0143 (5)
N2	0.52711 (16)	0.44491 (15)	0.29779 (12)	0.0126 (5)
C1	0.70896 (18)	0.17248 (18)	0.24020 (14)	0.0151 (6)
H1	0.6807	0.1179	0.2335	0.018*
C2	0.78920 (18)	0.18838 (18)	0.21566 (14)	0.0150 (6)
H2	0.8161	0.1453	0.1914	0.018*
C3	0.5260 (2)	0.41183 (17)	0.24253 (15)	0.0158 (6)
H3	0.5252	0.3501	0.2368	0.019*
C4	0.52588 (19)	0.46669 (17)	0.19470 (15)	0.0152 (6)
H4	0.5250	0.4428	0.1560	0.018*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Dy1	0.00587 (12)	0.00587 (12)	0.0051 (2)	−0.00030 (6)	0.000	0.000
Cl1	0.0138 (5)	0.0138 (5)	0.0061 (11)	0.000	0.000	0.000
Cl2	0.0263 (4)	0.0263 (4)	0.0316 (9)	−0.0106 (5)	0.0033 (3)	−0.0033 (3)
O1	0.0097 (8)	0.0235 (10)	0.0132 (12)	−0.0029 (7)	0.0045 (7)	−0.0042 (8)
O2	0.0247 (10)	0.0113 (8)	0.0100 (13)	−0.0020 (7)	−0.0023 (8)	0.0048 (7)
O3	0.0179 (11)	0.0433 (15)	0.0142 (15)	0.0047 (9)	−0.0040 (10)	−0.0023 (9)
O4	0.066 (3)	0.114 (5)	0.230 (7)	−0.010 (3)	0.097 (5)	−0.016 (5)
O5	0.076 (4)	0.099 (4)	0.212 (9)	0.003 (3)	−0.058 (5)	−0.076 (5)
N1	0.0113 (10)	0.0182 (10)	0.0134 (16)	−0.0011 (8)	0.0010 (9)	0.0001 (10)
N2	0.0149 (10)	0.0121 (10)	0.0108 (15)	−0.0003 (8)	−0.0013 (9)	0.0018 (9)
C1	0.0154 (12)	0.0159 (12)	0.0142 (17)	−0.0005 (9)	0.0008 (10)	−0.0029 (10)
C2	0.0137 (12)	0.0182 (13)	0.0130 (17)	−0.0004 (9)	0.0006 (10)	−0.0040 (11)
C3	0.0193 (13)	0.0110 (11)	0.0169 (18)	−0.0022 (10)	−0.0026 (12)	0.0005 (10)
C4	0.0205 (13)	0.0116 (11)	0.0135 (17)	−0.0001 (10)	0.0006 (11)	0.0000 (10)

Geometric parameters (Å, º)

Dy1—O1^i	2.333 (2)	Cl2—O5^vi	1.380 (6)
Dy1—O1^ii	2.333 (2)	O1—N1	1.306 (3)
Dy1—O1	2.333 (2)	O2—N2	1.298 (3)
Dy1—O1^iii	2.333 (2)	N1—C1	1.358 (4)
Dy1—O2^i	2.3665 (19)	N1—C2^vii	1.358 (4)
Dy1—O2^ii	2.3665 (19)	N2—C3	1.351 (4)
Dy1—O2	2.3665 (19)	N2—C4^viii	1.359 (3)
Dy1—O2^iii	2.3665 (19)	C1—C2	1.366 (4)
Cl1—O3	1.440 (2)	C1—H1	0.9500
Cl1—O3^iv	1.440 (2)	C2—N1^vii	1.358 (4)
Cl1—O3^iii	1.440 (2)	C2—H2	0.9500
Cl1—O3^v	1.440 (2)	C3—C4	1.370 (4)
Cl2—O4^vi	1.355 (4)	C3—H3	0.9500
Cl2—O4	1.355 (4)	C4—N2^viii	1.359 (3)
Cl2—O5	1.380 (6)	C4—H4	0.9500
O1^i—Dy1—O1^ii	78.16 (11)	O3^iv—Cl1—O3^iii	109.92 (11)
O1^i—Dy1—O1	147.81 (10)	O3—Cl1—O3^v	109.92 (11)
O1^ii—Dy1—O1	111.03 (11)	O3^iv—Cl1—O3^v	108.6 (2)
O1^i—Dy1—O1^iii	111.03 (11)	O3^iii—Cl1—O3^v	109.91 (11)
O1^ii—Dy1—O1^iii	147.81 (10)	O4^vi—Cl2—O4	109.3 (6)
O1—Dy1—O1^iii	78.16 (11)	O4^vi—Cl2—O5	114.0 (4)
O1^i—Dy1—O2^i	80.49 (7)	O4—Cl2—O5	109.9 (5)
O1^ii—Dy1—O2^i	72.64 (7)	O4^vi—Cl2—O5^vi	109.9 (5)
O1—Dy1—O2^i	73.66 (7)	O4—Cl2—O5^vi	114.0 (4)
O1^iii—Dy1—O2^i	138.16 (7)	O5—Cl2—O5^vi	99.7 (8)
O1^i—Dy1—O2^ii	72.64 (7)	N1—O1—Dy1	142.21 (18)
O1^ii—Dy1—O2^ii	80.49 (7)	N2—O2—Dy1	141.19 (17)
O1—Dy1—O2^ii	138.16 (7)	O1—N1—C1	119.1 (2)
O1^iii—Dy1—O2^ii	73.66 (7)	O1—N1—C2^vii	121.3 (2)
O2^i—Dy1—O2^ii	145.25 (11)	C1—N1—C2^vii	119.5 (2)
O1^i—Dy1—O2	73.66 (7)	O2—N2—C3	121.7 (2)
O1^ii—Dy1—O2	138.16 (7)	O2—N2—C4^viii	119.2 (3)
O1—Dy1—O2	80.49 (7)	C3—N2—C4^viii	119.1 (3)
O1^iii—Dy1—O2	72.64 (7)	N1—C1—C2	120.4 (3)
O2^i—Dy1—O2	72.71 (10)	N1—C1—H1	119.8
O2^ii—Dy1—O2	118.40 (10)	C2—C1—H1	119.8
O1^i—Dy1—O2^iii	138.16 (7)	N1^vii—C2—C1	120.1 (3)
O1^ii—Dy1—O2^iii	73.66 (7)	N1^vii—C2—H2	120.0
O1—Dy1—O2^iii	72.64 (7)	C1—C2—H2	120.0
O1^iii—Dy1—O2^iii	80.49 (7)	N2—C3—C4	120.4 (2)
O2^i—Dy1—O2^iii	118.40 (10)	N2—C3—H3	119.8
O2^ii—Dy1—O2^iii	72.71 (10)	C4—C3—H3	119.8
O2—Dy1—O2^iii	145.25 (11)	N2^viii—C4—C3	120.5 (3)
O3—Cl1—O3^iv	109.91 (11)	N2^viii—C4—H4	119.8
O3—Cl1—O3^iii	108.6 (2)	C3—C4—H4	119.8

Symmetry codes: (i) y+1/4, x−1/4, −z+3/4; (ii) −y+3/4, −x+3/4, −z+3/4; (iii) −x+1, −y+1/2, z; (iv) −y+3/4, x−1/4, −z+1/4; (v) y+1/4, −x+3/4, −z+1/4; (vi) y+3/4, x−3/4, −z+1/4; (vii) −x+3/2, −y+1/2, −z+1/2; (viii) x, −y+1, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2···O2^vii	0.95	2.52	3.293 (4)	138
C2—H2···O5	0.95	2.40	3.168 (6)	137
C3—H3···O1	0.95	2.60	3.329 (4)	134
C3—H3···O3	0.95	2.47	3.234 (4)	138
C4—H4···O3^iv	0.95	2.37	3.245 (4)	153

Symmetry codes: (iv) −y+3/4, x−1/4, −z+1/4; (vii) −x+3/2, −y+1/2, −z+1/2.