In the title complex, [Gd(
L)
2(CHO
2)(H
2O)
3] (
L− = 4-formyl-2-methoxyphenolate anion, C
8H
7O
3), the Gd
III ion occupies a site with mirror symmetry and assumes a bicapped triangular prismatic coordination environment defined by four O atoms from two
L− ligands, three O atoms from three coordinated water molecules and one O atom from a formate group. The formate group and one water molecule lie on a mirror plane. A three-dimensional network is formed by O—H
O hydrogen-bond interactions.
Supporting information
CCDC reference: 255473
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.017
- wR factor = 0.044
- Data-to-parameter ratio = 14.9
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for C9
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Triaquaformatobis(4-formyl-2-methoxyphenolato)gadolinium(III)
top
Crystal data top
[Gd(C8H7O3)2(CHO2)(H2O)3] | F(000) = 1100 |
Mr = 558.59 | Dx = 1.949 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 17301 reflections |
a = 7.7843 (16) Å | θ = 3.3–27.5° |
b = 21.977 (4) Å | µ = 3.54 mm−1 |
c = 11.129 (2) Å | T = 293 K |
V = 1903.9 (6) Å3 | Prism, pale yellow |
Z = 4 | 0.39 × 0.25 × 0.19 mm |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 2237 independent reflections |
Radiation source: fine-focus sealed tube | 2159 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
Detector resolution: 10 pixels mm-1 | θmax = 27.5°, θmin = 3.2° |
ω scans | h = −10→10 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −28→28 |
Tmin = 0.359, Tmax = 0.510 | l = −13→14 |
17409 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.017 | Hydrogen site location: difmap (O-H) and geom (C-H) |
wR(F2) = 0.044 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0254P)2 + 2.2018P] where P = (Fo2 + 2Fc2)/3 |
2237 reflections | (Δ/σ)max = 0.001 |
150 parameters | Δρmax = 0.50 e Å−3 |
6 restraints | Δρmin = −0.37 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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Gd1 | 0.324050 (16) | 0.2500 | 0.455973 (11) | 0.01622 (5) | |
O1W | 0.1781 (2) | 0.31586 (7) | 0.31772 (16) | 0.0372 (4) | |
H1W1 | 0.134 (4) | 0.3100 (12) | 0.2488 (16) | 0.056* | |
H1W2 | 0.176 (4) | 0.3539 (6) | 0.333 (3) | 0.056* | |
O2W | 0.4753 (3) | 0.2500 | 0.64021 (19) | 0.0303 (5) | |
H2W1 | 0.430 (4) | 0.2500 | 0.7088 (17) | 0.045* | |
H2W2 | 0.5838 (13) | 0.2500 | 0.646 (3) | 0.045* | |
O1 | 0.31359 (18) | 0.35831 (8) | 0.55350 (13) | 0.0251 (3) | |
O2 | 0.5443 (2) | 0.31496 (6) | 0.40391 (13) | 0.0257 (3) | |
O3 | 0.8292 (2) | 0.55705 (8) | 0.64785 (18) | 0.0415 (4) | |
O4 | 0.0715 (3) | 0.2500 | 0.5605 (2) | 0.0312 (5) | |
O5 | −0.1819 (3) | 0.2500 | 0.6462 (2) | 0.0597 (10) | |
C1 | 0.1949 (3) | 0.37867 (12) | 0.6432 (3) | 0.0398 (6) | |
H1A | 0.2462 | 0.3746 | 0.7213 | 0.060* | |
H1B | 0.0924 | 0.3545 | 0.6395 | 0.060* | |
H1C | 0.1665 | 0.4206 | 0.6290 | 0.060* | |
C2 | 0.4680 (3) | 0.38923 (9) | 0.54789 (17) | 0.0216 (4) | |
C3 | 0.5859 (3) | 0.36402 (9) | 0.46459 (17) | 0.0219 (4) | |
C4 | 0.7458 (3) | 0.39324 (11) | 0.4504 (2) | 0.0291 (5) | |
H4 | 0.8263 | 0.3773 | 0.3973 | 0.035* | |
C5 | 0.7837 (3) | 0.44508 (10) | 0.5143 (2) | 0.0289 (5) | |
H5 | 0.8893 | 0.4641 | 0.5031 | 0.035* | |
C6 | 0.6658 (3) | 0.46969 (10) | 0.5957 (2) | 0.0257 (4) | |
C7 | 0.5063 (3) | 0.44091 (9) | 0.61220 (19) | 0.0243 (4) | |
H7 | 0.4270 | 0.4567 | 0.6663 | 0.029* | |
C8 | 0.6988 (3) | 0.52644 (11) | 0.6579 (2) | 0.0318 (5) | |
H8 | 0.6141 | 0.5407 | 0.7097 | 0.038* | |
C9 | −0.0897 (4) | 0.2500 | 0.5576 (3) | 0.0296 (7) | |
H9 | −0.1425 | 0.2500 | 0.4826 | 0.036* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Gd1 | 0.01487 (8) | 0.01819 (8) | 0.01558 (8) | 0.000 | 0.00079 (5) | 0.000 |
O1W | 0.0578 (12) | 0.0215 (8) | 0.0323 (9) | −0.0014 (7) | −0.0243 (8) | 0.0030 (7) |
O2W | 0.0193 (10) | 0.0513 (13) | 0.0203 (10) | 0.000 | −0.0017 (8) | 0.000 |
O1 | 0.0206 (8) | 0.0275 (8) | 0.0272 (8) | −0.0025 (6) | 0.0043 (6) | −0.0084 (6) |
O2 | 0.0278 (8) | 0.0236 (7) | 0.0258 (7) | −0.0069 (6) | 0.0086 (6) | −0.0056 (6) |
O3 | 0.0452 (11) | 0.0282 (8) | 0.0510 (11) | −0.0107 (7) | −0.0101 (8) | −0.0051 (8) |
O4 | 0.0194 (11) | 0.0367 (12) | 0.0375 (12) | 0.000 | 0.0069 (9) | 0.000 |
O5 | 0.0193 (12) | 0.135 (3) | 0.0244 (13) | 0.000 | 0.0024 (10) | 0.000 |
C1 | 0.0302 (12) | 0.0396 (13) | 0.0495 (15) | −0.0043 (10) | 0.0157 (11) | −0.0189 (12) |
C2 | 0.0203 (9) | 0.0217 (9) | 0.0226 (9) | −0.0011 (8) | −0.0017 (8) | 0.0002 (7) |
C3 | 0.0237 (10) | 0.0206 (9) | 0.0215 (9) | −0.0027 (8) | 0.0004 (8) | 0.0012 (7) |
C4 | 0.0247 (11) | 0.0280 (11) | 0.0347 (12) | −0.0034 (9) | 0.0059 (9) | −0.0022 (9) |
C5 | 0.0242 (10) | 0.0247 (10) | 0.0379 (12) | −0.0060 (8) | −0.0030 (9) | 0.0025 (9) |
C6 | 0.0295 (11) | 0.0201 (9) | 0.0276 (10) | −0.0026 (8) | −0.0081 (8) | 0.0007 (8) |
C7 | 0.0251 (10) | 0.0243 (9) | 0.0236 (9) | 0.0023 (8) | −0.0025 (8) | −0.0025 (8) |
C8 | 0.0376 (13) | 0.0256 (10) | 0.0323 (12) | −0.0013 (9) | −0.0083 (9) | −0.0027 (9) |
C9 | 0.0229 (15) | 0.0415 (18) | 0.0243 (14) | 0.000 | 0.0006 (12) | 0.000 |
Geometric parameters (Å, º) top
Gd1—O4 | 2.284 (2) | O2W—H2W2 | 0.84 (2) |
Gd1—O2 | 2.3053 (15) | C1—H1A | 0.9600 |
Gd1—O2W | 2.364 (2) | C1—H1B | 0.9600 |
Gd1—O1W | 2.3986 (16) | C1—H1C | 0.9600 |
Gd1—O1 | 2.6174 (17) | C2—C7 | 1.375 (3) |
O3—C8 | 1.223 (3) | C2—C3 | 1.417 (3) |
C9—O4 | 1.255 (4) | C3—C4 | 1.409 (3) |
C9—O5 | 1.220 (4) | C4—C5 | 1.375 (3) |
Gd1—O2i | 2.3053 (15) | C4—H4 | 0.9300 |
Gd1—O1Wi | 2.3986 (16) | C5—C6 | 1.399 (3) |
Gd1—O1i | 2.6174 (17) | C5—H5 | 0.9300 |
O1—C2 | 1.382 (3) | C6—C7 | 1.406 (3) |
O1—C1 | 1.432 (3) | C6—C8 | 1.450 (3) |
O1W—H1W1 | 0.85 (3) | C7—H7 | 0.9300 |
O1W—H1W2 | 0.85 (3) | C8—H8 | 0.9300 |
O2—C3 | 1.313 (2) | C9—H9 | 0.9300 |
O2W—H2W1 | 0.84 (3) | | |
| | | |
O1—Gd1—O1i | 130.86 (7) | O3—C8—C6 | 125.2 (2) |
O1Wi—Gd1—O1 | 143.13 (5) | O3—C8—H8 | 117.4 |
O1W—Gd1—O1 | 72.69 (6) | O4—Gd1—O1i | 76.24 (4) |
O1Wi—Gd1—O1W | 74.23 (8) | O4—Gd1—O1W | 85.34 (7) |
O2—Gd1—O1 | 64.16 (5) | O4—Gd1—O2i | 140.19 (4) |
O2i—Gd1—O1 | 133.67 (5) | O4—C9—H9 | 117.7 |
O2—Gd1—O2i | 76.53 (8) | O5—C9—O4 | 124.6 (3) |
O2—Gd1—O2W | 81.23 (6) | O5—C9—H9 | 117.7 |
O2—Gd1—O1Wi | 124.39 (6) | C1—O1—Gd1 | 126.40 (14) |
O2i—Gd1—O1Wi | 79.49 (6) | C2—O1—C1 | 116.03 (17) |
O2W—Gd1—O1Wi | 142.39 (4) | C2—O1—Gd1 | 113.66 (12) |
O2W—Gd1—O1 | 69.87 (4) | C2—C7—C6 | 119.7 (2) |
O4—Gd1—O1 | 76.24 (4) | C2—C7—H7 | 120.2 |
O4—Gd1—O1Wi | 85.34 (7) | C3—O2—Gd1 | 124.25 (13) |
O4—Gd1—O2 | 140.19 (4) | C3—C4—H4 | 119.7 |
O4—Gd1—O2W | 89.27 (8) | C4—C3—C2 | 117.84 (19) |
Gd1—O1W—H1W1 | 132.8 (18) | C4—C5—C6 | 121.0 (2) |
Gd1—O1W—H1W2 | 118.1 (18) | C4—C5—H5 | 119.5 |
Gd1—O2W—H2W1 | 125 (2) | C5—C4—C3 | 120.6 (2) |
Gd1—O2W—H2W2 | 124 (2) | C5—C4—H4 | 119.7 |
O1—C1—H1A | 109.5 | C5—C6—C7 | 119.4 (2) |
O1—C1—H1B | 109.5 | C5—C6—C8 | 121.7 (2) |
O1—C2—C3 | 113.60 (17) | C6—C5—H5 | 119.5 |
O1—C1—H1C | 109.5 | C6—C7—H7 | 120.2 |
O1Wi—Gd1—O1i | 72.69 (6) | C6—C8—H8 | 117.4 |
O1W—Gd1—O1i | 143.13 (5) | C7—C2—O1 | 124.83 (19) |
O2—Gd1—O1i | 133.67 (5) | C7—C2—C3 | 121.5 (2) |
O2i—Gd1—O1i | 64.16 (5) | C7—C6—C8 | 118.8 (2) |
O2i—Gd1—O2W | 81.23 (6) | C9—O4—Gd1 | 147.9 (2) |
O2—Gd1—O1W | 79.49 (6) | H1A—C1—H1B | 109.5 |
O2i—Gd1—O1W | 124.39 (6) | H1A—C1—H1C | 109.5 |
O2—C3—C4 | 122.29 (19) | H1B—C1—H1C | 109.5 |
O2—C3—C2 | 119.87 (19) | H1W1—O1W—H1W2 | 108.7 (15) |
O2W—Gd1—O1W | 142.39 (4) | H2W1—O2W—H2W2 | 110.8 (17) |
O2W—Gd1—O1i | 69.87 (4) | | |
| | | |
Gd1—O1—C2—C3 | 15.8 (2) | O2i—Gd1—O1—C2 | 17.76 (16) |
Gd1—O1—C2—C7 | −166.46 (16) | O2i—Gd1—O2—C3 | −136.76 (14) |
Gd1—O2—C3—C4 | 162.56 (16) | O2—Gd1—O4—C9 | 104.69 (9) |
Gd1—O2—C3—C2 | −17.4 (3) | O2i—Gd1—O4—C9 | −104.69 (9) |
Gd1—O4—C9—O5 | 180.0 | O2—C3—C4—C5 | 179.0 (2) |
O1i—Gd1—O1—C1 | −47.3 (2) | O2W—Gd1—O1—C1 | −84.0 (2) |
O1i—Gd1—O1—C2 | 109.42 (13) | O2W—Gd1—O1—C2 | 72.69 (13) |
O1—Gd1—O2—C3 | 18.06 (15) | O2W—Gd1—O2—C3 | −53.76 (16) |
O1i—Gd1—O2—C3 | −104.80 (16) | O2W—Gd1—O4—C9 | 180.000 (1) |
O1—Gd1—O4—C9 | 110.56 (4) | O4—Gd1—O1—C1 | 10.35 (19) |
O1i—Gd1—O4—C9 | −110.56 (4) | O4—Gd1—O1—C2 | 167.04 (14) |
O1—C2—C7—C6 | −177.69 (19) | O4—Gd1—O2—C3 | 24.4 (2) |
O1—C2—C3—O2 | −1.5 (3) | C1—O1—C2—C3 | 175.0 (2) |
O1—C2—C3—C4 | 178.56 (19) | C1—O1—C2—C7 | −7.2 (3) |
O1Wi—Gd1—O1—C1 | 72.6 (2) | C2—C3—C4—C5 | −1.0 (3) |
O1W—Gd1—O1—C1 | 99.70 (19) | C3—C2—C7—C6 | −0.1 (3) |
O1Wi—Gd1—O1—C2 | −130.73 (14) | C3—C4—C5—C6 | 0.7 (4) |
O1W—Gd1—O1—C2 | −103.61 (14) | C4—C5—C6—C7 | −0.1 (3) |
O1Wi—Gd1—O2—C3 | 156.28 (15) | C4—C5—C6—C8 | −175.8 (2) |
O1W—Gd1—O2—C3 | 93.80 (16) | C5—C6—C7—C2 | −0.2 (3) |
O1Wi—Gd1—O4—C9 | −37.26 (4) | C5—C6—C8—O3 | −1.3 (4) |
O1W—Gd1—O4—C9 | 37.26 (4) | C7—C2—C3—O2 | −179.34 (19) |
O2—Gd1—O1—C1 | −173.8 (2) | C7—C2—C3—C4 | 0.7 (3) |
O2i—Gd1—O1—C1 | −138.93 (18) | C7—C6—C8—O3 | −177.1 (2) |
O2—Gd1—O1—C2 | −17.13 (12) | C8—C6—C7—C2 | 175.67 (19) |
Symmetry code: (i) x, −y+1/2, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2ii | 0.85 (3) | 1.84 (3) | 2.677 (2) | 168 (3) |
O1W—H1W2···O3iii | 0.85 (3) | 1.97 (2) | 2.820 (2) | 175 (3) |
O2W—H2W1···O5iv | 0.84 (3) | 1.83 (3) | 2.673 (4) | 177 (3) |
O2W—H2W2···O5v | 0.84 (2) | 1.82 (2) | 2.669 (3) | 176 (3) |
Symmetry codes: (ii) x−1/2, y, −z+1/2; (iii) −x+1, −y+1, −z+1; (iv) x+1/2, y, −z+3/2; (v) x+1, y, z. |