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The title three-dimensional coordination network, {[Ho(C4H4N2O2)4](ClO4)3}n, is isostructural to that of other lanthanides. The Ho+3 cation lies on a fourfold roto-inversion axis. It is coordinated in a distorted square anti-prismatic 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) (110) and inter­act with the coordination network through C—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536810031831/zl2300sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536810031831/zl2300Isup2.hkl
Contains datablock I

CCDC reference: 792275

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.035
  • wR factor = 0.103
  • Data-to-parameter ratio = 17.3

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      ..       2.35 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.
PLAT430_ALERT_2_A Short Inter D...A Contact  O3     ..  O3      ..       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.
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      ..       2.30 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      ..       2.12 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 PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O2 .. 2.77 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      ..       2.81 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  O2     ..  O2      ..       2.80 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       3.38 eA-3
PLAT973_ALERT_2_B Large Calcd. Positive Residual Density on    Ho1       1.55 eA-3

Alert level C PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 24 PLAT971_ALERT_2_C Large Calcd. Non-Metal Positive Residual Density 1.81 eA-3 PLAT971_ALERT_2_C Large Calcd. Non-Metal Positive Residual Density 1.60 eA-3 PLAT972_ALERT_2_C Large Calcd. Non-Metal Negative Residual Density -1.73 eA-3 PLAT972_ALERT_2_C Large Calcd. Non-Metal Negative Residual Density -1.51 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 43 PLAT952_ALERT_1_C Reported and Calculated Lmax Values Differ by .. 4
Alert level G REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 30.51 From the CIF: _reflns_number_total 1906 From the CIF: _diffrn_reflns_limit_ max hkl 21. 21. 28. From the CIF: _diffrn_reflns_limit_ min hkl -7. -20. -27. 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      ..       2.89 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      ..       2.89 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      ..       2.37 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  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      ..       2.72 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  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      ..       2.71 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.
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 10 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 40 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 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Comment top

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. 2010a), Dy (Quinn-Elmore et al. 2010b), Ho (this publication), and Er (Buchner et al. 2010), 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 the first article of this series by Quinn-Elmore et al. (2010a).

Related literature top

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

Experimental top

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 Ho(ClO4)3 (0.160 ml of a 0.0860 M solution, 0.0139 mmol) was diluted with methanol (0.840 ml)and CH2Cl2 (2.5 ml). The pyrazine N,N'-dioxide solution was layered over the Ho(ClO4)3 solution, and the two solutions were allowed to slowly mix. Orange plate-like crystals formed upon the slow evaporation of the resultant solution.

Refinement top

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

Structure description top

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. 2010a), Dy (Quinn-Elmore et al. 2010b), Ho (this publication), and Er (Buchner et al. 2010), 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 the first article of this series by Quinn-Elmore et al. (2010a).

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

Computing details top

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 top
[Figure 1] Fig. 1. The coordination environment of the Ho+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')holmium(III)] tris(perchlorate)] top
Crystal data top
[Ho(C4H4N2O2)4](ClO4)3Dx = 2.307 Mg m3
Mr = 911.65Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/acdCell parameters from 4928 reflections
Hall symbol: -I 4bd 2cθ = 2.6–30.5°
a = 15.2302 (4) ŵ = 3.43 mm1
c = 22.6334 (12) ÅT = 100 K
V = 5250.0 (3) Å3Plate, orange
Z = 80.37 × 0.32 × 0.17 mm
F(000) = 3568
Data collection top
Bruker SMART APEX CCD
diffractometer
1906 independent reflections
Radiation source: fine-focus sealed tube1585 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
ω scansθmax = 30.5°, θmin = 2.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 721
Tmin = 0.292, Tmax = 0.558k = 2021
10709 measured reflectionsl = 2728
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.103H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0554P)2 + 37.1849P]
where P = (Fo2 + 2Fc2)/3
1906 reflections(Δ/σ)max < 0.001
110 parametersΔρmax = 3.23 e Å3
0 restraintsΔρmin = 1.76 e Å3
Crystal data top
[Ho(C4H4N2O2)4](ClO4)3Z = 8
Mr = 911.65Mo Kα radiation
Tetragonal, I41/acdµ = 3.43 mm1
a = 15.2302 (4) ÅT = 100 K
c = 22.6334 (12) Å0.37 × 0.32 × 0.17 mm
V = 5250.0 (3) Å3
Data collection top
Bruker SMART APEX CCD
diffractometer
1906 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
1585 reflections with I > 2σ(I)
Tmin = 0.292, Tmax = 0.558Rint = 0.025
10709 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0350 restraints
wR(F2) = 0.103H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0554P)2 + 37.1849P]
where P = (Fo2 + 2Fc2)/3
1906 reflectionsΔρmax = 3.23 e Å3
110 parametersΔρmin = 1.76 e Å3
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
xyzUiso*/Ueq
Ho10.50000.25000.37500.00486 (12)
Cl10.50000.25000.12500.0107 (4)
Cl20.72659 (6)0.02341 (6)0.12500.0279 (3)
O10.59106 (13)0.21881 (15)0.29529 (10)0.0149 (4)
O20.53202 (15)0.39424 (13)0.34396 (10)0.0145 (4)
O30.57646 (17)0.24391 (17)0.16195 (12)0.0249 (6)
O40.6466 (4)0.0166 (5)0.1510 (4)0.137 (3)
O50.7914 (4)0.0059 (4)0.1660 (4)0.126 (3)
N10.66932 (17)0.23422 (18)0.27425 (13)0.0135 (5)
N20.52691 (17)0.44463 (16)0.29771 (12)0.0125 (5)
C10.70854 (19)0.17233 (19)0.24034 (14)0.0149 (6)
H10.68000.11780.23360.018*
C20.78932 (19)0.18805 (19)0.21558 (14)0.0145 (6)
H20.81630.14480.19140.017*
C30.5262 (2)0.41170 (19)0.24238 (14)0.0149 (6)
H30.52590.34990.23660.018*
C40.5259 (2)0.46676 (19)0.19448 (15)0.0150 (6)
H40.52490.44300.15570.018*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ho10.00537 (13)0.00537 (13)0.0038 (2)0.00033 (6)0.0000.000
Cl10.0132 (5)0.0132 (5)0.0058 (10)0.0000.0000.000
Cl20.0261 (4)0.0261 (4)0.0315 (8)0.0103 (5)0.0037 (3)0.0037 (3)
O10.0093 (9)0.0224 (11)0.0129 (11)0.0028 (8)0.0047 (8)0.0037 (8)
O20.0242 (11)0.0106 (9)0.0088 (12)0.0021 (8)0.0029 (8)0.0043 (7)
O30.0177 (12)0.0432 (16)0.0138 (14)0.0043 (9)0.0044 (10)0.0029 (10)
O40.066 (4)0.116 (5)0.228 (8)0.013 (3)0.098 (5)0.016 (5)
O50.078 (4)0.094 (4)0.205 (9)0.002 (3)0.059 (5)0.072 (5)
N10.0112 (11)0.0188 (11)0.0106 (15)0.0002 (9)0.0020 (9)0.0003 (10)
N20.0147 (11)0.0114 (10)0.0114 (14)0.0003 (9)0.0016 (9)0.0027 (9)
C10.0151 (13)0.0162 (13)0.0132 (16)0.0013 (10)0.0014 (10)0.0032 (11)
C20.0139 (13)0.0183 (13)0.0113 (16)0.0003 (10)0.0014 (10)0.0023 (11)
C30.0195 (14)0.0112 (12)0.0140 (17)0.0018 (10)0.0018 (12)0.0000 (10)
C40.0192 (13)0.0123 (12)0.0137 (16)0.0003 (11)0.0005 (11)0.0007 (10)
Geometric parameters (Å, º) top
Ho1—O1i2.325 (2)Cl2—O5vi1.381 (6)
Ho1—O1ii2.325 (2)O1—N11.305 (3)
Ho1—O12.325 (2)O2—N21.300 (3)
Ho1—O1iii2.325 (2)N1—C11.354 (4)
Ho1—O2i2.357 (2)N1—C2vii1.361 (4)
Ho1—O2ii2.357 (2)N2—C31.349 (4)
Ho1—O22.357 (2)N2—C4viii1.361 (4)
Ho1—O2iii2.357 (2)C1—C21.373 (4)
Cl1—O31.437 (3)C1—H10.9500
Cl1—O3iv1.437 (3)C2—N1vii1.361 (4)
Cl1—O3iii1.437 (3)C2—H20.9500
Cl1—O3v1.437 (3)C3—C41.371 (4)
Cl2—O4vi1.357 (4)C3—H30.9500
Cl2—O41.357 (4)C4—N2viii1.361 (4)
Cl2—O51.381 (6)C4—H40.9500
O1i—Ho1—O1ii78.19 (11)O3iv—Cl1—O3iii109.81 (11)
O1i—Ho1—O1147.80 (10)O3—Cl1—O3v109.81 (11)
O1ii—Ho1—O1111.01 (12)O3iv—Cl1—O3v108.8 (2)
O1i—Ho1—O1iii111.01 (12)O3iii—Cl1—O3v109.80 (11)
O1ii—Ho1—O1iii147.80 (10)O4vi—Cl2—O4109.0 (6)
O1—Ho1—O1iii78.19 (11)O4vi—Cl2—O5114.2 (4)
O1i—Ho1—O2i80.55 (8)O4—Cl2—O5109.6 (5)
O1ii—Ho1—O2i72.64 (7)O4vi—Cl2—O5vi109.6 (5)
O1—Ho1—O2i73.60 (7)O4—Cl2—O5vi114.2 (4)
O1iii—Ho1—O2i138.15 (7)O5—Cl2—O5vi100.2 (8)
O1i—Ho1—O2ii72.64 (7)N1—O1—Ho1142.32 (19)
O1ii—Ho1—O2ii80.55 (8)N2—O2—Ho1141.03 (18)
O1—Ho1—O2ii138.15 (7)O1—N1—C1119.0 (3)
O1iii—Ho1—O2ii73.60 (7)O1—N1—C2vii121.2 (3)
O2i—Ho1—O2ii145.32 (11)C1—N1—C2vii119.8 (3)
O1i—Ho1—O273.60 (7)O2—N2—C3121.9 (2)
O1ii—Ho1—O2138.15 (7)O2—N2—C4viii118.8 (3)
O1—Ho1—O280.55 (8)C3—N2—C4viii119.3 (3)
O1iii—Ho1—O272.64 (7)N1—C1—C2120.3 (3)
O2i—Ho1—O272.73 (11)N1—C1—H1119.8
O2ii—Ho1—O2118.32 (11)C2—C1—H1119.8
O1i—Ho1—O2iii138.15 (7)N1vii—C2—C1119.8 (3)
O1ii—Ho1—O2iii73.60 (7)N1vii—C2—H2120.1
O1—Ho1—O2iii72.64 (7)C1—C2—H2120.1
O1iii—Ho1—O2iii80.55 (8)N2—C3—C4120.4 (3)
O2i—Ho1—O2iii118.32 (11)N2—C3—H3119.8
O2ii—Ho1—O2iii72.73 (11)C4—C3—H3119.8
O2—Ho1—O2iii145.33 (11)N2viii—C4—C3120.3 (3)
O3—Cl1—O3iv109.80 (11)N2viii—C4—H4119.9
O3—Cl1—O3iii108.8 (2)C3—C4—H4119.9
Symmetry codes: (i) y+1/4, x1/4, z+3/4; (ii) y+3/4, x+3/4, z+3/4; (iii) x+1, y+1/2, z; (iv) y+3/4, x1/4, z+1/4; (v) y+1/4, x+3/4, z+1/4; (vi) y+3/4, x3/4, 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) top
D—H···AD—HH···AD···AD—H···A
C2—H2···O2vii0.952.523.285 (4)138
C2—H2···O50.952.403.161 (7)137
C3—H3···O10.952.603.323 (4)134
C3—H3···O30.952.463.230 (4)138
C4—H4···O3iv0.952.363.234 (4)153
Symmetry codes: (iv) y+3/4, x1/4, z+1/4; (vii) x+3/2, y+1/2, z+1/2.

Experimental details

Crystal data
Chemical formula[Ho(C4H4N2O2)4](ClO4)3
Mr911.65
Crystal system, space groupTetragonal, I41/acd
Temperature (K)100
a, c (Å)15.2302 (4), 22.6334 (12)
V3)5250.0 (3)
Z8
Radiation typeMo Kα
µ (mm1)3.43
Crystal size (mm)0.37 × 0.32 × 0.17
Data collection
DiffractometerBruker SMART APEX CCD
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.292, 0.558
No. of measured, independent and
observed [I > 2σ(I)] reflections
10709, 1906, 1585
Rint0.025
(sin θ/λ)max1)0.714
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.035, 0.103, 1.04
No. of reflections1906
No. of parameters110
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0554P)2 + 37.1849P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)3.23, 1.76

Computer programs: SMART (Bruker, 2007), SAINT-Plus (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C2—H2···O2i0.952.523.285 (4)138.0
C2—H2···O50.952.403.161 (7)137.3
C3—H3···O10.952.603.323 (4)133.6
C3—H3···O30.952.463.230 (4)138.0
C4—H4···O3ii0.952.363.234 (4)152.6
Symmetry codes: (i) x+3/2, y+1/2, z+1/2; (ii) y+3/4, x1/4, z+1/4.
 

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