In the title compound, [Gd2(C8H4O4)3(C3H7NO)2(H2O)2]n, the central GdIII atom is nine-coordinated by seven O atoms from benzene-1,4-dicarboxylate (1,4-BDC) ligands, one dimethylformamide and one water molecule in a distorted tricapped trigonal–prism coordination. The 1,4-BDC ligands link the GdIII atoms, forming a three-dimensional structure. All aromatic rings are located on centres of inversion. The water molecule forms hydrogen bonds to carboxylate groups.
Supporting information
CCDC reference: 613596
Key indicators
- Single-crystal X-ray study
- T = 292 K
- Mean (C-C) = 0.004 Å
- R factor = 0.017
- wR factor = 0.042
- Data-to-parameter ratio = 16.4
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.14 Ratio
| Author Response: maybe due to the librational and rotational behavior of the
methyl groups in DMF molecules.
|
PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.56 Ratio
| Author Response: maybe due to the librational and rotational behavior of the
methyl groups in DMF molecules.
|
Alert level B
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for N1
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT213_ALERT_2_C Atom C15 has ADP max/min Ratio ............. 3.80 prolat
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.01
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C14
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C15
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.23 Ratio
2 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
10 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
5 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
4 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXTL.
Poly[diaqua-µ
4-benzene-1,4-dicarboxylato-di-µ
2-benzene-1,4-dicarboxylato-
bis(
N,
N'-dimethylformamide)digadolinium(III)]
top
Crystal data top
[Gd2(C8H4O4)3(C3H7NO)2(H2O)2] | Z = 1 |
Mr = 989.06 | F(000) = 480 |
Triclinic, P1 | Dx = 1.957 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.6066 (17) Å | Cell parameters from 7950 reflections |
b = 10.156 (2) Å | θ = 3.0–27.5° |
c = 11.161 (2) Å | µ = 4.00 mm−1 |
α = 65.26 (3)° | T = 292 K |
β = 71.76 (3)° | Block, colourless |
γ = 78.68 (3)° | 0.33 × 0.31 × 0.29 mm |
V = 839.1 (4) Å3 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 3806 independent reflections |
Radiation source: rotor target | 3626 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.016 |
Detector resolution: 10.0 pixels mm-1 | θmax = 27.5°, θmin = 3.2° |
ω scans | h = −11→11 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −12→13 |
Tmin = 0.253, Tmax = 0.316 | l = −13→14 |
8319 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: inferred from neighbouring sites |
wR(F2) = 0.042 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.09 | w = 1/[σ2(Fo2) + (0.021P)2 + 0.6587P] where P = (Fo2 + 2Fc2)/3 |
3806 reflections | (Δ/σ)max = 0.003 |
232 parameters | Δρmax = 0.70 e Å−3 |
0 restraints | Δρmin = −0.66 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 | |
C1 | 0.0684 (3) | 0.2348 (2) | 0.5526 (2) | 0.0207 (4) | |
C2 | 0.0326 (3) | 0.1144 (2) | 0.5236 (2) | 0.0207 (4) | |
C3 | 0.0428 (3) | 0.1312 (3) | 0.3915 (3) | 0.0266 (5) | |
H3 | 0.0713 | 0.2186 | 0.3189 | 0.032* | |
C4 | 0.0100 (3) | 0.0164 (3) | 0.3687 (3) | 0.0271 (5) | |
H4 | 0.0167 | 0.0274 | 0.2803 | 0.033* | |
C5 | 0.3254 (3) | 0.2320 (2) | 0.8199 (2) | 0.0224 (5) | |
C6 | 0.4174 (3) | 0.1110 (2) | 0.9111 (2) | 0.0230 (5) | |
C7 | 0.5801 (3) | 0.0691 (3) | 0.8640 (3) | 0.0327 (6) | |
H7 | 0.6347 | 0.1151 | 0.7727 | 0.039* | |
C8 | 0.3380 (3) | 0.0411 (3) | 1.0482 (3) | 0.0340 (6) | |
H8 | 0.2287 | 0.0688 | 1.0811 | 0.041* | |
C9 | −0.1789 (3) | 0.4611 (2) | 0.8309 (2) | 0.0211 (4) | |
C10 | −0.3452 (3) | 0.4823 (3) | 0.9176 (2) | 0.0225 (5) | |
C11 | −0.4747 (3) | 0.4133 (3) | 0.9270 (3) | 0.0297 (5) | |
H11 | −0.4575 | 0.3549 | 0.8777 | 0.036* | |
C12 | −0.3704 (3) | 0.5698 (3) | 0.9910 (3) | 0.0284 (5) | |
H12 | −0.2840 | 0.6166 | 0.9852 | 0.034* | |
C13 | 0.2424 (5) | 0.6720 (3) | 0.7523 (4) | 0.0443 (8) | |
H13 | 0.1506 | 0.6525 | 0.8266 | 0.053* | |
C14 | 0.4844 (9) | 0.7975 (7) | 0.6216 (7) | 0.126 (3) | |
H14A | 0.5395 | 0.8720 | 0.6198 | 0.189* | |
H14B | 0.4566 | 0.8284 | 0.5364 | 0.189* | |
H14C | 0.5553 | 0.7097 | 0.6350 | 0.189* | |
C15 | 0.2894 (9) | 0.8514 (5) | 0.8222 (7) | 0.121 (3) | |
H15A | 0.3697 | 0.9192 | 0.7943 | 0.182* | |
H15B | 0.2836 | 0.7846 | 0.9146 | 0.182* | |
H15C | 0.1841 | 0.9032 | 0.8166 | 0.182* | |
N1 | 0.3361 (5) | 0.7709 (3) | 0.7323 (4) | 0.0669 (11) | |
O1 | 0.0362 (2) | 0.36646 (17) | 0.48056 (17) | 0.0233 (3) | |
O2 | 0.1311 (3) | 0.20219 (19) | 0.6491 (2) | 0.0353 (5) | |
O1W | 0.3181 (3) | 0.5427 (3) | 0.4320 (2) | 0.0378 (5) | |
O3 | 0.3978 (2) | 0.29960 (19) | 0.69548 (18) | 0.0277 (4) | |
O4 | 0.1783 (2) | 0.2650 (2) | 0.86895 (18) | 0.0304 (4) | |
O5 | −0.1569 (2) | 0.38106 (18) | 0.76416 (17) | 0.0238 (3) | |
O6 | −0.0631 (2) | 0.52337 (19) | 0.82501 (18) | 0.0263 (4) | |
O7 | 0.2694 (3) | 0.6039 (2) | 0.6784 (2) | 0.0381 (5) | |
Gd1 | 0.131860 (13) | 0.439754 (11) | 0.653288 (11) | 0.01689 (4) | |
HW11 | 0.394 (4) | 0.580 (3) | 0.405 (3) | 0.025* | |
HW12 | 0.287 (4) | 0.562 (3) | 0.374 (3) | 0.025* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0206 (11) | 0.0162 (10) | 0.0276 (11) | 0.0002 (8) | −0.0075 (9) | −0.0104 (9) |
C2 | 0.0217 (11) | 0.0146 (10) | 0.0284 (11) | −0.0001 (8) | −0.0092 (9) | −0.0093 (9) |
C3 | 0.0392 (15) | 0.0156 (10) | 0.0253 (12) | −0.0065 (9) | −0.0108 (10) | −0.0043 (9) |
C4 | 0.0402 (15) | 0.0204 (11) | 0.0238 (11) | −0.0040 (10) | −0.0112 (10) | −0.0086 (10) |
C5 | 0.0252 (12) | 0.0200 (10) | 0.0267 (11) | −0.0018 (9) | −0.0146 (10) | −0.0078 (9) |
C6 | 0.0260 (12) | 0.0188 (10) | 0.0267 (12) | 0.0001 (9) | −0.0147 (10) | −0.0064 (9) |
C7 | 0.0301 (14) | 0.0334 (13) | 0.0243 (12) | 0.0023 (10) | −0.0083 (10) | −0.0024 (11) |
C8 | 0.0236 (13) | 0.0372 (14) | 0.0308 (13) | 0.0068 (10) | −0.0090 (11) | −0.0058 (12) |
C9 | 0.0243 (12) | 0.0188 (10) | 0.0189 (10) | −0.0017 (8) | −0.0063 (9) | −0.0055 (9) |
C10 | 0.0234 (12) | 0.0236 (11) | 0.0208 (11) | −0.0026 (9) | −0.0040 (9) | −0.0097 (9) |
C11 | 0.0267 (13) | 0.0356 (13) | 0.0346 (13) | −0.0082 (10) | −0.0016 (10) | −0.0229 (11) |
C12 | 0.0238 (12) | 0.0344 (13) | 0.0339 (13) | −0.0084 (10) | −0.0022 (10) | −0.0206 (11) |
C13 | 0.058 (2) | 0.0279 (14) | 0.064 (2) | 0.0024 (13) | −0.0416 (17) | −0.0171 (14) |
C14 | 0.130 (6) | 0.087 (4) | 0.155 (6) | −0.077 (4) | −0.053 (5) | 0.003 (4) |
C15 | 0.225 (7) | 0.040 (2) | 0.185 (6) | 0.038 (3) | −0.175 (6) | −0.057 (3) |
N1 | 0.102 (3) | 0.0282 (13) | 0.101 (3) | −0.0028 (15) | −0.077 (2) | −0.0178 (16) |
O1 | 0.0298 (9) | 0.0135 (7) | 0.0275 (8) | 0.0015 (6) | −0.0106 (7) | −0.0078 (7) |
O2 | 0.0546 (13) | 0.0197 (8) | 0.0452 (11) | 0.0049 (8) | −0.0354 (10) | −0.0127 (8) |
O1W | 0.0250 (10) | 0.0611 (14) | 0.0239 (9) | −0.0181 (9) | −0.0064 (8) | −0.0064 (9) |
O3 | 0.0247 (9) | 0.0274 (9) | 0.0264 (9) | −0.0016 (7) | −0.0114 (7) | −0.0025 (7) |
O4 | 0.0264 (9) | 0.0346 (10) | 0.0258 (9) | 0.0062 (7) | −0.0114 (7) | −0.0076 (8) |
O5 | 0.0230 (9) | 0.0265 (8) | 0.0253 (8) | −0.0038 (6) | −0.0046 (7) | −0.0137 (7) |
O6 | 0.0238 (9) | 0.0303 (9) | 0.0305 (9) | −0.0055 (7) | −0.0048 (7) | −0.0171 (8) |
O7 | 0.0390 (11) | 0.0335 (10) | 0.0532 (12) | −0.0096 (8) | −0.0177 (10) | −0.0202 (10) |
Gd1 | 0.01681 (6) | 0.01540 (6) | 0.02011 (6) | −0.00065 (4) | −0.00800 (4) | −0.00633 (4) |
Geometric parameters (Å, º) top
C1—O2 | 1.247 (3) | C11—H11 | 0.9300 |
C1—O1 | 1.267 (3) | C12—C11iii | 1.387 (4) |
C1—C2 | 1.496 (3) | C12—H12 | 0.9300 |
C1—Gd1 | 2.947 (2) | C13—O7 | 1.228 (4) |
C2—C4i | 1.387 (3) | C13—N1 | 1.314 (4) |
C2—C3 | 1.387 (3) | C13—H13 | 0.9300 |
C3—C4 | 1.388 (3) | C14—N1 | 1.448 (8) |
C3—H3 | 0.9300 | C14—H14A | 0.9600 |
C4—C2i | 1.387 (3) | C14—H14B | 0.9600 |
C4—H4 | 0.9300 | C14—H14C | 0.9600 |
C5—O4 | 1.252 (3) | C15—N1 | 1.463 (6) |
C5—O3 | 1.271 (3) | C15—H15A | 0.9600 |
C5—C6 | 1.499 (3) | C15—H15B | 0.9600 |
C5—Gd1 | 2.822 (3) | C15—H15C | 0.9600 |
C6—C7 | 1.383 (4) | O1—Gd1iv | 2.4436 (19) |
C6—C8 | 1.392 (4) | O1—Gd1 | 2.7175 (18) |
C7—C8ii | 1.384 (4) | O2—Gd1 | 2.4343 (18) |
C7—H7 | 0.9300 | O1W—Gd1 | 2.404 (2) |
C8—C7ii | 1.384 (4) | O1W—HW11 | 0.73 (3) |
C8—H8 | 0.9300 | O1W—HW12 | 0.72 (3) |
C9—O6 | 1.253 (3) | O3—Gd1 | 2.5143 (19) |
C9—O5 | 1.268 (3) | O4—Gd1 | 2.4189 (19) |
C9—C10 | 1.490 (3) | O5—Gd1 | 2.4703 (19) |
C9—Gd1 | 2.818 (3) | O6—Gd1 | 2.4493 (19) |
C10—C11 | 1.384 (4) | O7—Gd1 | 2.3729 (19) |
C10—C12 | 1.388 (3) | Gd1—O1iv | 2.4436 (19) |
C11—C12iii | 1.387 (4) | | |
| | | |
O2—C1—O1 | 121.0 (2) | C5—O4—Gd1 | 95.14 (15) |
O2—C1—C2 | 118.3 (2) | C9—O5—Gd1 | 92.10 (14) |
O1—C1—C2 | 120.7 (2) | C9—O6—Gd1 | 93.47 (14) |
O2—C1—Gd1 | 54.07 (12) | C13—O7—Gd1 | 137.2 (2) |
O1—C1—Gd1 | 67.12 (12) | O7—Gd1—O1W | 76.41 (8) |
C2—C1—Gd1 | 171.22 (16) | O7—Gd1—O4 | 86.94 (8) |
C4i—C2—C3 | 119.9 (2) | O1W—Gd1—O4 | 131.44 (7) |
C4i—C2—C1 | 118.9 (2) | O7—Gd1—O2 | 148.78 (7) |
C3—C2—C1 | 121.2 (2) | O1W—Gd1—O2 | 97.10 (9) |
C2—C3—C4 | 119.5 (2) | O4—Gd1—O2 | 74.52 (7) |
C2—C3—H3 | 120.3 | O7—Gd1—O1iv | 93.53 (7) |
C4—C3—H3 | 120.3 | O1W—Gd1—O1iv | 75.90 (7) |
C2i—C4—C3 | 120.6 (2) | O4—Gd1—O1iv | 151.47 (6) |
C2i—C4—H4 | 119.7 | O2—Gd1—O1iv | 114.76 (6) |
C3—C4—H4 | 119.7 | O7—Gd1—O6 | 73.86 (7) |
O4—C5—O3 | 121.4 (2) | O1W—Gd1—O6 | 138.23 (8) |
O4—C5—C6 | 118.9 (2) | O4—Gd1—O6 | 75.39 (7) |
O3—C5—C6 | 119.8 (2) | O2—Gd1—O6 | 123.21 (7) |
O4—C5—Gd1 | 58.63 (12) | O1iv—Gd1—O6 | 77.36 (6) |
O3—C5—Gd1 | 63.01 (12) | O7—Gd1—O5 | 126.74 (7) |
C6—C5—Gd1 | 174.47 (16) | O1W—Gd1—O5 | 141.71 (7) |
C7—C6—C8 | 118.9 (2) | O4—Gd1—O5 | 84.01 (7) |
C7—C6—C5 | 122.0 (2) | O2—Gd1—O5 | 76.82 (7) |
C8—C6—C5 | 119.1 (2) | O1iv—Gd1—O5 | 72.89 (7) |
C6—C7—C8ii | 120.4 (2) | O6—Gd1—O5 | 53.04 (6) |
C6—C7—H7 | 119.8 | O7—Gd1—O3 | 76.20 (7) |
C8ii—C7—H7 | 119.8 | O1W—Gd1—O3 | 78.70 (7) |
C7ii—C8—C6 | 120.7 (3) | O4—Gd1—O3 | 52.93 (7) |
C7ii—C8—H8 | 119.6 | O2—Gd1—O3 | 72.58 (7) |
C6—C8—H8 | 119.6 | O1iv—Gd1—O3 | 154.23 (6) |
O6—C9—O5 | 121.2 (2) | O6—Gd1—O3 | 120.70 (6) |
O6—C9—C10 | 119.1 (2) | O5—Gd1—O3 | 132.12 (6) |
O5—C9—C10 | 119.7 (2) | O7—Gd1—O1 | 147.14 (7) |
O6—C9—Gd1 | 60.18 (12) | O1W—Gd1—O1 | 73.51 (7) |
O5—C9—Gd1 | 61.17 (12) | O4—Gd1—O1 | 123.21 (6) |
C10—C9—Gd1 | 176.09 (16) | O2—Gd1—O1 | 49.90 (6) |
C11—C10—C12 | 119.7 (2) | O1iv—Gd1—O1 | 66.62 (6) |
C11—C10—C9 | 120.2 (2) | O6—Gd1—O1 | 122.76 (6) |
C12—C10—C9 | 120.1 (2) | O5—Gd1—O1 | 74.09 (6) |
C10—C11—C12iii | 120.8 (2) | O3—Gd1—O1 | 110.02 (6) |
C10—C11—H11 | 119.6 | O7—Gd1—C9 | 100.03 (8) |
C12iii—C11—H11 | 119.6 | O1W—Gd1—C9 | 147.76 (8) |
C11iii—C12—C10 | 119.4 (2) | O4—Gd1—C9 | 79.48 (7) |
C11iii—C12—H12 | 120.3 | O2—Gd1—C9 | 100.94 (8) |
C10—C12—H12 | 120.3 | O1iv—Gd1—C9 | 72.34 (7) |
O7—C13—N1 | 123.7 (4) | O6—Gd1—C9 | 26.35 (6) |
O7—C13—H13 | 118.2 | O5—Gd1—C9 | 26.73 (6) |
N1—C13—H13 | 118.2 | O3—Gd1—C9 | 132.25 (6) |
N1—C14—H14A | 109.5 | O1—Gd1—C9 | 98.36 (6) |
N1—C14—H14B | 109.5 | O7—Gd1—C5 | 82.13 (7) |
H14A—C14—H14B | 109.5 | O1W—Gd1—C5 | 105.48 (8) |
N1—C14—H14C | 109.5 | O4—Gd1—C5 | 26.23 (7) |
H14A—C14—H14C | 109.5 | O2—Gd1—C5 | 70.08 (7) |
H14B—C14—H14C | 109.5 | O1iv—Gd1—C5 | 174.92 (6) |
N1—C15—H15A | 109.5 | O6—Gd1—C5 | 98.80 (7) |
N1—C15—H15B | 109.5 | O5—Gd1—C5 | 107.58 (7) |
H15A—C15—H15B | 109.5 | O3—Gd1—C5 | 26.78 (7) |
N1—C15—H15C | 109.5 | O1—Gd1—C5 | 118.44 (6) |
H15A—C15—H15C | 109.5 | C9—Gd1—C5 | 105.71 (7) |
H15B—C15—H15C | 109.5 | O7—Gd1—C1 | 160.36 (7) |
C13—N1—C14 | 119.1 (4) | O1W—Gd1—C1 | 86.16 (8) |
C13—N1—C15 | 119.6 (5) | O4—Gd1—C1 | 98.20 (7) |
C14—N1—C15 | 121.3 (4) | O2—Gd1—C1 | 24.50 (6) |
C1—O1—Gd1iv | 152.36 (16) | O1iv—Gd1—C1 | 90.86 (6) |
C1—O1—Gd1 | 87.44 (14) | O6—Gd1—C1 | 125.76 (6) |
Gd1iv—O1—Gd1 | 113.38 (6) | O5—Gd1—C1 | 72.81 (7) |
C1—O2—Gd1 | 101.43 (14) | O3—Gd1—C1 | 91.74 (7) |
Gd1—O1W—HW11 | 136 (3) | O1—Gd1—C1 | 25.44 (6) |
Gd1—O1W—HW12 | 117 (3) | C9—Gd1—C1 | 99.54 (7) |
HW11—O1W—HW12 | 104 (3) | C5—Gd1—C1 | 94.10 (7) |
C5—O3—Gd1 | 90.21 (15) | | |
Symmetry codes: (i) −x, −y, −z+1; (ii) −x+1, −y, −z+2; (iii) −x−1, −y+1, −z+2; (iv) −x, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—HW11···O3v | 0.73 (3) | 2.10 (3) | 2.832 (3) | 173 (3) |
O1W—HW12···O5iv | 0.72 (3) | 2.01 (3) | 2.717 (3) | 169 (3) |
Symmetry codes: (iv) −x, −y+1, −z+1; (v) −x+1, −y+1, −z+1. |