Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean
(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
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.
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).
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).
Poly[[tetrakis(µ
2-pyrazine
N,
N'-dioxide-
κ2O:
O')holmium(III)]
tris(perchlorate)]
top
Crystal data top
[Ho(C4H4N2O2)4](ClO4)3 | Dx = 2.307 Mg m−3 |
Mr = 911.65 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I41/acd | Cell parameters from 4928 reflections |
Hall symbol: -I 4bd 2c | θ = 2.6–30.5° |
a = 15.2302 (4) Å | µ = 3.43 mm−1 |
c = 22.6334 (12) Å | T = 100 K |
V = 5250.0 (3) Å3 | Plate, orange |
Z = 8 | 0.37 × 0.32 × 0.17 mm |
F(000) = 3568 | |
Data collection top
Bruker SMART APEX CCD diffractometer | 1906 independent reflections |
Radiation source: fine-focus sealed tube | 1585 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
ω scans | θmax = 30.5°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −7→21 |
Tmin = 0.292, Tmax = 0.558 | k = −20→21 |
10709 measured reflections | l = −27→28 |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.103 | H-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 parameters | Δρmax = 3.23 e Å−3 |
0 restraints | Δρmin = −1.76 e Å−3 |
Crystal data top
[Ho(C4H4N2O2)4](ClO4)3 | Z = 8 |
Mr = 911.65 | Mo Kα radiation |
Tetragonal, I41/acd | µ = 3.43 mm−1 |
a = 15.2302 (4) Å | T = 100 K |
c = 22.6334 (12) Å | 0.37 × 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 = 0.558 | Rint = 0.025 |
10709 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.035 | 0 restraints |
wR(F2) = 0.103 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0554P)2 + 37.1849P] where P = (Fo2 + 2Fc2)/3 |
1906 reflections | Δρmax = 3.23 e Å−3 |
110 parameters | Δρmin = −1.76 e Å−3 |
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 | Uiso*/Ueq | |
Ho1 | 0.5000 | 0.2500 | 0.3750 | 0.00486 (12) | |
Cl1 | 0.5000 | 0.2500 | 0.1250 | 0.0107 (4) | |
Cl2 | 0.72659 (6) | −0.02341 (6) | 0.1250 | 0.0279 (3) | |
O1 | 0.59106 (13) | 0.21881 (15) | 0.29529 (10) | 0.0149 (4) | |
O2 | 0.53202 (15) | 0.39424 (13) | 0.34396 (10) | 0.0145 (4) | |
O3 | 0.57646 (17) | 0.24391 (17) | 0.16195 (12) | 0.0249 (6) | |
O4 | 0.6466 (4) | −0.0166 (5) | 0.1510 (4) | 0.137 (3) | |
O5 | 0.7914 (4) | −0.0059 (4) | 0.1660 (4) | 0.126 (3) | |
N1 | 0.66932 (17) | 0.23422 (18) | 0.27425 (13) | 0.0135 (5) | |
N2 | 0.52691 (17) | 0.44463 (16) | 0.29771 (12) | 0.0125 (5) | |
C1 | 0.70854 (19) | 0.17233 (19) | 0.24034 (14) | 0.0149 (6) | |
H1 | 0.6800 | 0.1178 | 0.2336 | 0.018* | |
C2 | 0.78932 (19) | 0.18805 (19) | 0.21558 (14) | 0.0145 (6) | |
H2 | 0.8163 | 0.1448 | 0.1914 | 0.017* | |
C3 | 0.5262 (2) | 0.41170 (19) | 0.24238 (14) | 0.0149 (6) | |
H3 | 0.5259 | 0.3499 | 0.2366 | 0.018* | |
C4 | 0.5259 (2) | 0.46676 (19) | 0.19448 (15) | 0.0150 (6) | |
H4 | 0.5249 | 0.4430 | 0.1557 | 0.018* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ho1 | 0.00537 (13) | 0.00537 (13) | 0.0038 (2) | −0.00033 (6) | 0.000 | 0.000 |
Cl1 | 0.0132 (5) | 0.0132 (5) | 0.0058 (10) | 0.000 | 0.000 | 0.000 |
Cl2 | 0.0261 (4) | 0.0261 (4) | 0.0315 (8) | −0.0103 (5) | 0.0037 (3) | −0.0037 (3) |
O1 | 0.0093 (9) | 0.0224 (11) | 0.0129 (11) | −0.0028 (8) | 0.0047 (8) | −0.0037 (8) |
O2 | 0.0242 (11) | 0.0106 (9) | 0.0088 (12) | −0.0021 (8) | −0.0029 (8) | 0.0043 (7) |
O3 | 0.0177 (12) | 0.0432 (16) | 0.0138 (14) | 0.0043 (9) | −0.0044 (10) | −0.0029 (10) |
O4 | 0.066 (4) | 0.116 (5) | 0.228 (8) | −0.013 (3) | 0.098 (5) | −0.016 (5) |
O5 | 0.078 (4) | 0.094 (4) | 0.205 (9) | 0.002 (3) | −0.059 (5) | −0.072 (5) |
N1 | 0.0112 (11) | 0.0188 (11) | 0.0106 (15) | −0.0002 (9) | 0.0020 (9) | 0.0003 (10) |
N2 | 0.0147 (11) | 0.0114 (10) | 0.0114 (14) | −0.0003 (9) | −0.0016 (9) | 0.0027 (9) |
C1 | 0.0151 (13) | 0.0162 (13) | 0.0132 (16) | −0.0013 (10) | 0.0014 (10) | −0.0032 (11) |
C2 | 0.0139 (13) | 0.0183 (13) | 0.0113 (16) | −0.0003 (10) | 0.0014 (10) | −0.0023 (11) |
C3 | 0.0195 (14) | 0.0112 (12) | 0.0140 (17) | −0.0018 (10) | −0.0018 (12) | 0.0000 (10) |
C4 | 0.0192 (13) | 0.0123 (12) | 0.0137 (16) | −0.0003 (11) | 0.0005 (11) | 0.0007 (10) |
Geometric parameters (Å, º) top
Ho1—O1i | 2.325 (2) | Cl2—O5vi | 1.381 (6) |
Ho1—O1ii | 2.325 (2) | O1—N1 | 1.305 (3) |
Ho1—O1 | 2.325 (2) | O2—N2 | 1.300 (3) |
Ho1—O1iii | 2.325 (2) | N1—C1 | 1.354 (4) |
Ho1—O2i | 2.357 (2) | N1—C2vii | 1.361 (4) |
Ho1—O2ii | 2.357 (2) | N2—C3 | 1.349 (4) |
Ho1—O2 | 2.357 (2) | N2—C4viii | 1.361 (4) |
Ho1—O2iii | 2.357 (2) | C1—C2 | 1.373 (4) |
Cl1—O3 | 1.437 (3) | C1—H1 | 0.9500 |
Cl1—O3iv | 1.437 (3) | C2—N1vii | 1.361 (4) |
Cl1—O3iii | 1.437 (3) | C2—H2 | 0.9500 |
Cl1—O3v | 1.437 (3) | C3—C4 | 1.371 (4) |
Cl2—O4vi | 1.357 (4) | C3—H3 | 0.9500 |
Cl2—O4 | 1.357 (4) | C4—N2viii | 1.361 (4) |
Cl2—O5 | 1.381 (6) | C4—H4 | 0.9500 |
| | | |
O1i—Ho1—O1ii | 78.19 (11) | O3iv—Cl1—O3iii | 109.81 (11) |
O1i—Ho1—O1 | 147.80 (10) | O3—Cl1—O3v | 109.81 (11) |
O1ii—Ho1—O1 | 111.01 (12) | O3iv—Cl1—O3v | 108.8 (2) |
O1i—Ho1—O1iii | 111.01 (12) | O3iii—Cl1—O3v | 109.80 (11) |
O1ii—Ho1—O1iii | 147.80 (10) | O4vi—Cl2—O4 | 109.0 (6) |
O1—Ho1—O1iii | 78.19 (11) | O4vi—Cl2—O5 | 114.2 (4) |
O1i—Ho1—O2i | 80.55 (8) | O4—Cl2—O5 | 109.6 (5) |
O1ii—Ho1—O2i | 72.64 (7) | O4vi—Cl2—O5vi | 109.6 (5) |
O1—Ho1—O2i | 73.60 (7) | O4—Cl2—O5vi | 114.2 (4) |
O1iii—Ho1—O2i | 138.15 (7) | O5—Cl2—O5vi | 100.2 (8) |
O1i—Ho1—O2ii | 72.64 (7) | N1—O1—Ho1 | 142.32 (19) |
O1ii—Ho1—O2ii | 80.55 (8) | N2—O2—Ho1 | 141.03 (18) |
O1—Ho1—O2ii | 138.15 (7) | O1—N1—C1 | 119.0 (3) |
O1iii—Ho1—O2ii | 73.60 (7) | O1—N1—C2vii | 121.2 (3) |
O2i—Ho1—O2ii | 145.32 (11) | C1—N1—C2vii | 119.8 (3) |
O1i—Ho1—O2 | 73.60 (7) | O2—N2—C3 | 121.9 (2) |
O1ii—Ho1—O2 | 138.15 (7) | O2—N2—C4viii | 118.8 (3) |
O1—Ho1—O2 | 80.55 (8) | C3—N2—C4viii | 119.3 (3) |
O1iii—Ho1—O2 | 72.64 (7) | N1—C1—C2 | 120.3 (3) |
O2i—Ho1—O2 | 72.73 (11) | N1—C1—H1 | 119.8 |
O2ii—Ho1—O2 | 118.32 (11) | C2—C1—H1 | 119.8 |
O1i—Ho1—O2iii | 138.15 (7) | N1vii—C2—C1 | 119.8 (3) |
O1ii—Ho1—O2iii | 73.60 (7) | N1vii—C2—H2 | 120.1 |
O1—Ho1—O2iii | 72.64 (7) | C1—C2—H2 | 120.1 |
O1iii—Ho1—O2iii | 80.55 (8) | N2—C3—C4 | 120.4 (3) |
O2i—Ho1—O2iii | 118.32 (11) | N2—C3—H3 | 119.8 |
O2ii—Ho1—O2iii | 72.73 (11) | C4—C3—H3 | 119.8 |
O2—Ho1—O2iii | 145.33 (11) | N2viii—C4—C3 | 120.3 (3) |
O3—Cl1—O3iv | 109.80 (11) | N2viii—C4—H4 | 119.9 |
O3—Cl1—O3iii | 108.8 (2) | C3—C4—H4 | 119.9 |
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) top
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H2···O2vii | 0.95 | 2.52 | 3.285 (4) | 138 |
C2—H2···O5 | 0.95 | 2.40 | 3.161 (7) | 137 |
C3—H3···O1 | 0.95 | 2.60 | 3.323 (4) | 134 |
C3—H3···O3 | 0.95 | 2.46 | 3.230 (4) | 138 |
C4—H4···O3iv | 0.95 | 2.36 | 3.234 (4) | 153 |
Symmetry codes: (iv) −y+3/4, x−1/4, −z+1/4; (vii) −x+3/2, −y+1/2, −z+1/2. |
Experimental details
Crystal data |
Chemical formula | [Ho(C4H4N2O2)4](ClO4)3 |
Mr | 911.65 |
Crystal system, space group | Tetragonal, I41/acd |
Temperature (K) | 100 |
a, c (Å) | 15.2302 (4), 22.6334 (12) |
V (Å3) | 5250.0 (3) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 3.43 |
Crystal size (mm) | 0.37 × 0.32 × 0.17 |
|
Data collection |
Diffractometer | Bruker SMART APEX CCD |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.292, 0.558 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10709, 1906, 1585 |
Rint | 0.025 |
(sin θ/λ)max (Å−1) | 0.714 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.035, 0.103, 1.04 |
No. of reflections | 1906 |
No. of parameters | 110 |
H-atom treatment | H-atom parameters constrained |
| w = 1/[σ2(Fo2) + (0.0554P)2 + 37.1849P] where P = (Fo2 + 2Fc2)/3 |
Δρmax, Δρmin (e Å−3) | 3.23, −1.76 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H2···O2i | 0.95 | 2.52 | 3.285 (4) | 138.0 |
C2—H2···O5 | 0.95 | 2.40 | 3.161 (7) | 137.3 |
C3—H3···O1 | 0.95 | 2.60 | 3.323 (4) | 133.6 |
C3—H3···O3 | 0.95 | 2.46 | 3.230 (4) | 138.0 |
C4—H4···O3ii | 0.95 | 2.36 | 3.234 (4) | 152.6 |
Symmetry codes: (i) −x+3/2, −y+1/2, −z+1/2; (ii) −y+3/4, x−1/4, −z+1/4. |
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).