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The HoIII center in the title coordination polymer, {[Ho2(C4H4O4)3(H2O)2]·H2O}n, is nine-coordinated in a tricapped trigonal prism by eight O atoms, derived from six carboxylate groups and a water molecule. One of the independent succinate anions is located about a crystallographic center of inversion and the uncoordinated water molecule lies on a twofold axis. The crystal structure comprises edge-shared HoO9 polyhedra linked by succinate bridges, forming a three-dimensional network structure.
Supporting information
CCDC reference: 295067
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.006 Å
- R factor = 0.020
- wR factor = 0.049
- Data-to-parameter ratio = 15.6
checkCIF/PLATON results
No syntax errors found
Alert level C
CELLV02_ALERT_1_C The supplied cell volume s.u. differs from that
calculated from the cell parameter s.u.'s by > 2
Calculated cell volume su = 8.57
Cell volume su given = 6.00
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.78
PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.67 mm
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.40 Ratio
Alert level G
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 0.778
Tmax scaled 0.290 Tmin scaled 0.051
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
6 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 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
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: RAPID-AUTO (Rigaku ,2004); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
Poly[[diaqua-µ
6-succinato-di-µ
5-succinato-diholmium(III)] monohydrate]
top
Crystal data top
[Ho2(C4H4O4)3(H2O)2]·H2O | F(000) = 1376 |
Mr = 732.12 | Dx = 2.712 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 8491 reflections |
a = 19.852 (4) Å | θ = 3.0–27.5° |
b = 7.6723 (15) Å | µ = 8.84 mm−1 |
c = 13.800 (3) Å | T = 295 K |
β = 121.46 (3)° | Prism, yellow |
V = 1792.9 (6) Å3 | 0.67 × 0.23 × 0.14 mm |
Z = 4 | |
Data collection top
Rigaku R-AXIS RAPID IP area-detector diffractometer | 2058 independent reflections |
Radiation source: rotating anode | 2011 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
oscillation scans | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan (Jacobson, 1998) | h = −25→25 |
Tmin = 0.066, Tmax = 0.373 | k = −9→9 |
8553 measured reflections | l = −17→17 |
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)] = 0.020 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.049 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0139P)2 + 15.8528P] where P = (Fo2 + 2Fc2)/3 |
2058 reflections | (Δ/σ)max = 0.001 |
132 parameters | Δρmax = 0.92 e Å−3 |
0 restraints | Δρmin = −1.59 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 | 0.268916 (8) | 0.217620 (18) | 0.230019 (11) | 0.00885 (7) | |
O1W | 0.33298 (16) | 0.3880 (3) | 0.1523 (2) | 0.0192 (5) | |
H1A | 0.3233 | 0.4962 | 0.1396 | 0.023* | |
H1B | 0.3293 | 0.3492 | 0.0920 | 0.023* | |
O1 | 0.17158 (17) | 0.7362 (3) | 0.5283 (2) | 0.0182 (5) | |
O2 | 0.18728 (14) | 0.5174 (3) | 0.6376 (2) | 0.0163 (5) | |
O3 | 0.17989 (16) | 0.5268 (3) | 0.3411 (2) | 0.0201 (5) | |
O4 | 0.19710 (19) | 0.2451 (4) | 0.3246 (3) | 0.0232 (6) | |
O5 | 0.32311 (13) | 0.4827 (3) | 0.3393 (2) | 0.0146 (5) | |
O6 | 0.40612 (16) | 0.2702 (3) | 0.3790 (2) | 0.0203 (6) | |
C1 | 0.15305 (18) | 0.5847 (5) | 0.5384 (3) | 0.0115 (6) | |
C2 | 0.0906 (2) | 0.4836 (5) | 0.4377 (3) | 0.0153 (7) | |
H2A | 0.0651 | 0.5606 | 0.3724 | 0.018* | |
H2B | 0.0509 | 0.4449 | 0.4536 | 0.018* | |
C3 | 0.1230 (2) | 0.3249 (5) | 0.4077 (3) | 0.0169 (7) | |
H3A | 0.1564 | 0.2587 | 0.4764 | 0.020* | |
H3B | 0.0791 | 0.2507 | 0.3562 | 0.020* | |
C4 | 0.17016 (19) | 0.3706 (4) | 0.3529 (3) | 0.0122 (6) | |
C5 | 0.39427 (19) | 0.4243 (5) | 0.3927 (3) | 0.0128 (6) | |
C6 | 0.4601 (2) | 0.5446 (5) | 0.4695 (3) | 0.0237 (8) | |
H6A | 0.4496 | 0.5925 | 0.5254 | 0.028* | |
H6B | 0.4617 | 0.6407 | 0.4251 | 0.028* | |
O2W | 0.5000 | 0.4745 (15) | 0.2500 | 0.114 (3) | |
H2C | 0.4608 | 0.4201 | 0.2445 | 0.136* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ho1 | 0.01035 (9) | 0.00585 (11) | 0.01101 (9) | −0.00045 (5) | 0.00604 (7) | −0.00017 (5) |
O1W | 0.0298 (14) | 0.0121 (13) | 0.0242 (13) | −0.0027 (11) | 0.0200 (11) | −0.0026 (10) |
O1 | 0.0275 (14) | 0.0093 (12) | 0.0148 (12) | 0.0002 (11) | 0.0090 (11) | 0.0005 (9) |
O2 | 0.0168 (11) | 0.0175 (13) | 0.0109 (10) | −0.0023 (10) | 0.0047 (9) | 0.0028 (9) |
O3 | 0.0305 (14) | 0.0100 (12) | 0.0323 (14) | −0.0021 (11) | 0.0251 (12) | −0.0009 (10) |
O4 | 0.0356 (16) | 0.0113 (12) | 0.0382 (17) | 0.0001 (12) | 0.0300 (15) | −0.0016 (12) |
O5 | 0.0094 (10) | 0.0162 (13) | 0.0150 (11) | −0.0003 (10) | 0.0041 (9) | −0.0043 (9) |
O6 | 0.0137 (12) | 0.0115 (13) | 0.0263 (14) | −0.0005 (10) | 0.0038 (11) | −0.0007 (10) |
C1 | 0.0107 (14) | 0.0129 (16) | 0.0117 (14) | 0.0045 (13) | 0.0065 (12) | −0.0001 (12) |
C2 | 0.0142 (15) | 0.0186 (18) | 0.0132 (15) | 0.0001 (14) | 0.0073 (13) | −0.0024 (13) |
C3 | 0.0225 (17) | 0.0147 (17) | 0.0198 (16) | −0.0046 (15) | 0.0155 (14) | −0.0041 (14) |
C4 | 0.0149 (15) | 0.0077 (15) | 0.0151 (14) | −0.0021 (12) | 0.0086 (12) | −0.0015 (12) |
C5 | 0.0114 (15) | 0.0129 (16) | 0.0129 (14) | −0.0006 (13) | 0.0054 (12) | 0.0016 (12) |
C6 | 0.0110 (17) | 0.0168 (19) | 0.031 (2) | −0.0015 (15) | 0.0024 (15) | −0.0070 (16) |
O2W | 0.075 (5) | 0.130 (9) | 0.130 (8) | 0.000 | 0.050 (6) | 0.000 |
Geometric parameters (Å, º) top
Ho1—O1W | 2.429 (3) | O3—Ho1v | 2.276 (2) |
Ho1—O1i | 2.448 (3) | O4—C4 | 1.259 (4) |
Ho1—O2i | 2.496 (3) | O5—C5 | 1.286 (4) |
Ho1—O2ii | 2.385 (3) | O5—Ho1v | 2.383 (3) |
Ho1—O3iii | 2.276 (2) | O6—C5 | 1.239 (4) |
Ho1—O4 | 2.392 (3) | C1—C2 | 1.507 (5) |
Ho1—O5 | 2.423 (2) | C1—Ho1iv | 2.869 (3) |
Ho1—O5iii | 2.383 (3) | C2—C3 | 1.531 (5) |
Ho1—O6 | 2.442 (3) | C2—H2A | 0.9700 |
Ho1—C5 | 2.813 (3) | C2—H2B | 0.9700 |
Ho1—C1i | 2.869 (3) | C3—C4 | 1.520 (5) |
O1W—H1A | 0.8500 | C3—H3A | 0.9700 |
O1W—H1B | 0.8501 | C3—H3B | 0.9700 |
O1—C1 | 1.249 (4) | C5—C6 | 1.496 (5) |
O1—Ho1iv | 2.448 (3) | C6—C6vi | 1.514 (7) |
O2—C1 | 1.277 (4) | C6—H6A | 0.9700 |
O2—Ho1ii | 2.385 (3) | C6—H6B | 0.9700 |
O2—Ho1iv | 2.496 (3) | O2W—H2C | 0.8509 |
O3—C4 | 1.238 (4) | | |
| | | |
O3iii—Ho1—O5iii | 76.21 (9) | O6—Ho1—C1i | 133.94 (9) |
O3iii—Ho1—O2ii | 77.16 (9) | O1i—Ho1—C1i | 25.63 (9) |
O5iii—Ho1—O2ii | 68.42 (9) | O2i—Ho1—C1i | 26.38 (9) |
O3iii—Ho1—O4 | 145.01 (10) | C5—Ho1—C1i | 112.78 (10) |
O5iii—Ho1—O4 | 74.64 (9) | Ho1—O1W—H1A | 120.2 |
O2ii—Ho1—O4 | 74.41 (10) | Ho1—O1W—H1B | 116.5 |
O3iii—Ho1—O5 | 130.91 (9) | H1A—O1W—H1B | 104.2 |
O5iii—Ho1—O5 | 152.00 (3) | C1—O1—Ho1iv | 96.4 (2) |
O2ii—Ho1—O5 | 106.96 (9) | C1—O2—Ho1ii | 154.7 (2) |
O4—Ho1—O5 | 77.53 (9) | C1—O2—Ho1iv | 93.3 (2) |
O3iii—Ho1—O1W | 72.61 (9) | Ho1ii—O2—Ho1iv | 110.14 (9) |
O5iii—Ho1—O1W | 134.29 (8) | C4—O3—Ho1v | 144.6 (2) |
O2ii—Ho1—O1W | 132.81 (9) | C4—O4—Ho1 | 135.0 (2) |
O4—Ho1—O1W | 142.38 (9) | C5—O5—Ho1v | 151.2 (2) |
O5—Ho1—O1W | 70.04 (8) | C5—O5—Ho1 | 93.6 (2) |
O3iii—Ho1—O6 | 85.21 (10) | Ho1v—O5—Ho1 | 112.75 (9) |
O5iii—Ho1—O6 | 138.38 (8) | C5—O6—Ho1 | 93.9 (2) |
O2ii—Ho1—O6 | 71.30 (9) | O1—C1—O2 | 118.3 (3) |
O4—Ho1—O6 | 104.28 (11) | O1—C1—C2 | 121.6 (3) |
O5—Ho1—O6 | 53.10 (8) | O2—C1—C2 | 120.1 (3) |
O1W—Ho1—O6 | 70.84 (10) | O1—C1—Ho1iv | 57.98 (18) |
O3iii—Ho1—O1i | 82.40 (10) | O2—C1—Ho1iv | 60.27 (18) |
O5iii—Ho1—O1i | 70.63 (9) | C2—C1—Ho1iv | 178.6 (2) |
O2ii—Ho1—O1i | 137.42 (9) | C1—C2—C3 | 113.6 (3) |
O4—Ho1—O1i | 105.44 (11) | C1—C2—H2A | 108.9 |
O5—Ho1—O1i | 114.63 (9) | C3—C2—H2A | 108.9 |
O1W—Ho1—O1i | 72.81 (9) | C1—C2—H2B | 108.9 |
O6—Ho1—O1i | 143.61 (10) | C3—C2—H2B | 108.9 |
O3iii—Ho1—O2i | 128.35 (9) | H2A—C2—H2B | 107.7 |
O5iii—Ho1—O2i | 104.71 (9) | C4—C3—C2 | 113.9 (3) |
O2ii—Ho1—O2i | 152.54 (2) | C4—C3—H3A | 108.8 |
O4—Ho1—O2i | 78.13 (9) | C2—C3—H3A | 108.8 |
O5—Ho1—O2i | 66.01 (9) | C4—C3—H3B | 108.8 |
O1W—Ho1—O2i | 71.69 (9) | C2—C3—H3B | 108.8 |
O6—Ho1—O2i | 115.92 (9) | H3A—C3—H3B | 107.7 |
O1i—Ho1—O2i | 52.01 (8) | O3—C4—O4 | 125.4 (3) |
O3iii—Ho1—C5 | 107.36 (10) | O3—C4—C3 | 117.9 (3) |
O5iii—Ho1—C5 | 156.96 (9) | O4—C4—C3 | 116.7 (3) |
O2ii—Ho1—C5 | 89.87 (9) | O6—C5—O5 | 119.0 (3) |
O4—Ho1—C5 | 92.64 (10) | O6—C5—C6 | 122.1 (3) |
O5—Ho1—C5 | 27.14 (9) | O5—C5—C6 | 118.9 (3) |
O1W—Ho1—C5 | 66.43 (9) | O6—C5—Ho1 | 60.00 (18) |
O6—Ho1—C5 | 26.05 (9) | O5—C5—Ho1 | 59.28 (17) |
O1i—Ho1—C5 | 132.09 (9) | C6—C5—Ho1 | 174.3 (3) |
O2i—Ho1—C5 | 90.96 (9) | C5—C6—C6vi | 112.9 (4) |
O3iii—Ho1—C1i | 105.43 (10) | C5—C6—H6A | 109.0 |
O5iii—Ho1—C1i | 87.25 (9) | C6vi—C6—H6A | 109.0 |
O2ii—Ho1—C1i | 154.42 (9) | C5—C6—H6B | 109.0 |
O4—Ho1—C1i | 92.12 (10) | C6vi—C6—H6B | 109.0 |
O5—Ho1—C1i | 90.68 (9) | H6A—C6—H6B | 107.8 |
O1W—Ho1—C1i | 70.20 (9) | | |
Symmetry codes: (i) x, −y+1, z−1/2; (ii) −x+1/2, −y+1/2, −z+1; (iii) −x+1/2, y−1/2, −z+1/2; (iv) x, −y+1, z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1A···O4v | 0.85 | 2.06 | 2.857 (4) | 155 |
O1W—H1B···O1iii | 0.85 | 1.86 | 2.709 (4) | 172 |
O2W—H2C···O1W | 0.85 | 2.18 | 2.930 (4) | 147 |
Symmetry codes: (iii) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2. |
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