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In the title complex, [Gd(L)2(CHO2)(H2O)3] (L = 4-formyl-2-methoxy­phenolate anion, C8H7O3), the GdIII 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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804027205/hb6118sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804027205/hb6118Isup2.hkl
Contains datablock I

CCDC reference: 255473

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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

Computing details top

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 = 558.59Dx = 1.949 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 17301 reflections
a = 7.7843 (16) Åθ = 3.3–27.5°
b = 21.977 (4) ŵ = 3.54 mm1
c = 11.129 (2) ÅT = 293 K
V = 1903.9 (6) Å3Prism, pale yellow
Z = 40.39 × 0.25 × 0.19 mm
Data collection top
Rigaku R-AXIS RAPID
diffractometer
2237 independent reflections
Radiation source: fine-focus sealed tube2159 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
Detector resolution: 10 pixels mm-1θmax = 27.5°, θmin = 3.2°
ω scansh = 1010
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 2828
Tmin = 0.359, Tmax = 0.510l = 1314
17409 measured reflections
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)] = 0.017Hydrogen site location: difmap (O-H) and geom (C-H)
wR(F2) = 0.044H 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 parametersΔρmax = 0.50 e Å3
6 restraintsΔρmin = 0.37 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Gd10.324050 (16)0.25000.455973 (11)0.01622 (5)
O1W0.1781 (2)0.31586 (7)0.31772 (16)0.0372 (4)
H1W10.134 (4)0.3100 (12)0.2488 (16)0.056*
H1W20.176 (4)0.3539 (6)0.333 (3)0.056*
O2W0.4753 (3)0.25000.64021 (19)0.0303 (5)
H2W10.430 (4)0.25000.7088 (17)0.045*
H2W20.5838 (13)0.25000.646 (3)0.045*
O10.31359 (18)0.35831 (8)0.55350 (13)0.0251 (3)
O20.5443 (2)0.31496 (6)0.40391 (13)0.0257 (3)
O30.8292 (2)0.55705 (8)0.64785 (18)0.0415 (4)
O40.0715 (3)0.25000.5605 (2)0.0312 (5)
O50.1819 (3)0.25000.6462 (2)0.0597 (10)
C10.1949 (3)0.37867 (12)0.6432 (3)0.0398 (6)
H1A0.24620.37460.72130.060*
H1B0.09240.35450.63950.060*
H1C0.16650.42060.62900.060*
C20.4680 (3)0.38923 (9)0.54789 (17)0.0216 (4)
C30.5859 (3)0.36402 (9)0.46459 (17)0.0219 (4)
C40.7458 (3)0.39324 (11)0.4504 (2)0.0291 (5)
H40.82630.37730.39730.035*
C50.7837 (3)0.44508 (10)0.5143 (2)0.0289 (5)
H50.88930.46410.50310.035*
C60.6658 (3)0.46969 (10)0.5957 (2)0.0257 (4)
C70.5063 (3)0.44091 (9)0.61220 (19)0.0243 (4)
H70.42700.45670.66630.029*
C80.6988 (3)0.52644 (11)0.6579 (2)0.0318 (5)
H80.61410.54070.70970.038*
C90.0897 (4)0.25000.5576 (3)0.0296 (7)
H90.14250.25000.48260.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Gd10.01487 (8)0.01819 (8)0.01558 (8)0.0000.00079 (5)0.000
O1W0.0578 (12)0.0215 (8)0.0323 (9)0.0014 (7)0.0243 (8)0.0030 (7)
O2W0.0193 (10)0.0513 (13)0.0203 (10)0.0000.0017 (8)0.000
O10.0206 (8)0.0275 (8)0.0272 (8)0.0025 (6)0.0043 (6)0.0084 (6)
O20.0278 (8)0.0236 (7)0.0258 (7)0.0069 (6)0.0086 (6)0.0056 (6)
O30.0452 (11)0.0282 (8)0.0510 (11)0.0107 (7)0.0101 (8)0.0051 (8)
O40.0194 (11)0.0367 (12)0.0375 (12)0.0000.0069 (9)0.000
O50.0193 (12)0.135 (3)0.0244 (13)0.0000.0024 (10)0.000
C10.0302 (12)0.0396 (13)0.0495 (15)0.0043 (10)0.0157 (11)0.0189 (12)
C20.0203 (9)0.0217 (9)0.0226 (9)0.0011 (8)0.0017 (8)0.0002 (7)
C30.0237 (10)0.0206 (9)0.0215 (9)0.0027 (8)0.0004 (8)0.0012 (7)
C40.0247 (11)0.0280 (11)0.0347 (12)0.0034 (9)0.0059 (9)0.0022 (9)
C50.0242 (10)0.0247 (10)0.0379 (12)0.0060 (8)0.0030 (9)0.0025 (9)
C60.0295 (11)0.0201 (9)0.0276 (10)0.0026 (8)0.0081 (8)0.0007 (8)
C70.0251 (10)0.0243 (9)0.0236 (9)0.0023 (8)0.0025 (8)0.0025 (8)
C80.0376 (13)0.0256 (10)0.0323 (12)0.0013 (9)0.0083 (9)0.0027 (9)
C90.0229 (15)0.0415 (18)0.0243 (14)0.0000.0006 (12)0.000
Geometric parameters (Å, º) top
Gd1—O42.284 (2)O2W—H2W20.84 (2)
Gd1—O22.3053 (15)C1—H1A0.9600
Gd1—O2W2.364 (2)C1—H1B0.9600
Gd1—O1W2.3986 (16)C1—H1C0.9600
Gd1—O12.6174 (17)C2—C71.375 (3)
O3—C81.223 (3)C2—C31.417 (3)
C9—O41.255 (4)C3—C41.409 (3)
C9—O51.220 (4)C4—C51.375 (3)
Gd1—O2i2.3053 (15)C4—H40.9300
Gd1—O1Wi2.3986 (16)C5—C61.399 (3)
Gd1—O1i2.6174 (17)C5—H50.9300
O1—C21.382 (3)C6—C71.406 (3)
O1—C11.432 (3)C6—C81.450 (3)
O1W—H1W10.85 (3)C7—H70.9300
O1W—H1W20.85 (3)C8—H80.9300
O2—C31.313 (2)C9—H90.9300
O2W—H2W10.84 (3)
O1—Gd1—O1i130.86 (7)O3—C8—C6125.2 (2)
O1Wi—Gd1—O1143.13 (5)O3—C8—H8117.4
O1W—Gd1—O172.69 (6)O4—Gd1—O1i76.24 (4)
O1Wi—Gd1—O1W74.23 (8)O4—Gd1—O1W85.34 (7)
O2—Gd1—O164.16 (5)O4—Gd1—O2i140.19 (4)
O2i—Gd1—O1133.67 (5)O4—C9—H9117.7
O2—Gd1—O2i76.53 (8)O5—C9—O4124.6 (3)
O2—Gd1—O2W81.23 (6)O5—C9—H9117.7
O2—Gd1—O1Wi124.39 (6)C1—O1—Gd1126.40 (14)
O2i—Gd1—O1Wi79.49 (6)C2—O1—C1116.03 (17)
O2W—Gd1—O1Wi142.39 (4)C2—O1—Gd1113.66 (12)
O2W—Gd1—O169.87 (4)C2—C7—C6119.7 (2)
O4—Gd1—O176.24 (4)C2—C7—H7120.2
O4—Gd1—O1Wi85.34 (7)C3—O2—Gd1124.25 (13)
O4—Gd1—O2140.19 (4)C3—C4—H4119.7
O4—Gd1—O2W89.27 (8)C4—C3—C2117.84 (19)
Gd1—O1W—H1W1132.8 (18)C4—C5—C6121.0 (2)
Gd1—O1W—H1W2118.1 (18)C4—C5—H5119.5
Gd1—O2W—H2W1125 (2)C5—C4—C3120.6 (2)
Gd1—O2W—H2W2124 (2)C5—C4—H4119.7
O1—C1—H1A109.5C5—C6—C7119.4 (2)
O1—C1—H1B109.5C5—C6—C8121.7 (2)
O1—C2—C3113.60 (17)C6—C5—H5119.5
O1—C1—H1C109.5C6—C7—H7120.2
O1Wi—Gd1—O1i72.69 (6)C6—C8—H8117.4
O1W—Gd1—O1i143.13 (5)C7—C2—O1124.83 (19)
O2—Gd1—O1i133.67 (5)C7—C2—C3121.5 (2)
O2i—Gd1—O1i64.16 (5)C7—C6—C8118.8 (2)
O2i—Gd1—O2W81.23 (6)C9—O4—Gd1147.9 (2)
O2—Gd1—O1W79.49 (6)H1A—C1—H1B109.5
O2i—Gd1—O1W124.39 (6)H1A—C1—H1C109.5
O2—C3—C4122.29 (19)H1B—C1—H1C109.5
O2—C3—C2119.87 (19)H1W1—O1W—H1W2108.7 (15)
O2W—Gd1—O1W142.39 (4)H2W1—O2W—H2W2110.8 (17)
O2W—Gd1—O1i69.87 (4)
Gd1—O1—C2—C315.8 (2)O2i—Gd1—O1—C217.76 (16)
Gd1—O1—C2—C7166.46 (16)O2i—Gd1—O2—C3136.76 (14)
Gd1—O2—C3—C4162.56 (16)O2—Gd1—O4—C9104.69 (9)
Gd1—O2—C3—C217.4 (3)O2i—Gd1—O4—C9104.69 (9)
Gd1—O4—C9—O5180.0O2—C3—C4—C5179.0 (2)
O1i—Gd1—O1—C147.3 (2)O2W—Gd1—O1—C184.0 (2)
O1i—Gd1—O1—C2109.42 (13)O2W—Gd1—O1—C272.69 (13)
O1—Gd1—O2—C318.06 (15)O2W—Gd1—O2—C353.76 (16)
O1i—Gd1—O2—C3104.80 (16)O2W—Gd1—O4—C9180.000 (1)
O1—Gd1—O4—C9110.56 (4)O4—Gd1—O1—C110.35 (19)
O1i—Gd1—O4—C9110.56 (4)O4—Gd1—O1—C2167.04 (14)
O1—C2—C7—C6177.69 (19)O4—Gd1—O2—C324.4 (2)
O1—C2—C3—O21.5 (3)C1—O1—C2—C3175.0 (2)
O1—C2—C3—C4178.56 (19)C1—O1—C2—C77.2 (3)
O1Wi—Gd1—O1—C172.6 (2)C2—C3—C4—C51.0 (3)
O1W—Gd1—O1—C199.70 (19)C3—C2—C7—C60.1 (3)
O1Wi—Gd1—O1—C2130.73 (14)C3—C4—C5—C60.7 (4)
O1W—Gd1—O1—C2103.61 (14)C4—C5—C6—C70.1 (3)
O1Wi—Gd1—O2—C3156.28 (15)C4—C5—C6—C8175.8 (2)
O1W—Gd1—O2—C393.80 (16)C5—C6—C7—C20.2 (3)
O1Wi—Gd1—O4—C937.26 (4)C5—C6—C8—O31.3 (4)
O1W—Gd1—O4—C937.26 (4)C7—C2—C3—O2179.34 (19)
O2—Gd1—O1—C1173.8 (2)C7—C2—C3—C40.7 (3)
O2i—Gd1—O1—C1138.93 (18)C7—C6—C8—O3177.1 (2)
O2—Gd1—O1—C217.13 (12)C8—C6—C7—C2175.67 (19)
Symmetry code: (i) x, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O2ii0.85 (3)1.84 (3)2.677 (2)168 (3)
O1W—H1W2···O3iii0.85 (3)1.97 (2)2.820 (2)175 (3)
O2W—H2W1···O5iv0.84 (3)1.83 (3)2.673 (4)177 (3)
O2W—H2W2···O5v0.84 (2)1.82 (2)2.669 (3)176 (3)
Symmetry codes: (ii) x1/2, y, z+1/2; (iii) x+1, y+1, z+1; (iv) x+1/2, y, z+3/2; (v) x+1, y, z.
 

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