Poly[diaqua-μ₄-benzene-1,4-dicarboxyl­ato-di-μ₂-benzene-1,4-dicarboxyl­ato-bis­(N,N′-dimethyl­formamide)digadolinium(III)]

In the title compound, [Gd₂(C₈H₄O₄)₃(C₃H₇NO)₂(H₂O)₂]_n, the central Gd^III 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 Gd^III atoms, forming a three-dimensional structure. All aromatic rings are located on centres of inversion. The water mol­ecule forms hydrogen bonds to carboxyl­ate groups.

Key indicators

• Single-crystal X-ray study
• T = 292 K
• Mean [sigma](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

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Computing details

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-µ₄-benzene-1,4-dicarboxylato-di-µ₂-benzene-1,4-dicarboxylato- bis(N,N'-dimethylformamide)digadolinium(III)]

Crystal data

[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) Å^3

Data collection

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

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.017	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.042	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	w = 1/[σ^2(Fo^2) + (0.021P)^2 + 0.6587P] where P = (Fo^2 + 2Fc^2)/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

C1—O2	1.247 (3)	C11—H11	0.9300
C1—O1	1.267 (3)	C12—C11^iii	1.387 (4)
C1—C2	1.496 (3)	C12—H12	0.9300
C1—Gd1	2.947 (2)	C13—O7	1.228 (4)
C2—C4^i	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—C2^i	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—Gd1^iv	2.4436 (19)
C6—C8	1.392 (4)	O1—Gd1	2.7175 (18)
C7—C8^ii	1.384 (4)	O2—Gd1	2.4343 (18)
C7—H7	0.9300	O1W—Gd1	2.404 (2)
C8—C7^ii	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—O1^iv	2.4436 (19)
C11—C12^iii	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)
C4^i—C2—C3	119.9 (2)	O1W—Gd1—O4	131.44 (7)
C4^i—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—O1^iv	93.53 (7)
C4—C3—H3	120.3	O1W—Gd1—O1^iv	75.90 (7)
C2^i—C4—C3	120.6 (2)	O4—Gd1—O1^iv	151.47 (6)
C2^i—C4—H4	119.7	O2—Gd1—O1^iv	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)	O1^iv—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)	O1^iv—Gd1—O5	72.89 (7)
C6—C7—C8^ii	120.4 (2)	O6—Gd1—O5	53.04 (6)
C6—C7—H7	119.8	O7—Gd1—O3	76.20 (7)
C8^ii—C7—H7	119.8	O1W—Gd1—O3	78.70 (7)
C7^ii—C8—C6	120.7 (3)	O4—Gd1—O3	52.93 (7)
C7^ii—C8—H8	119.6	O2—Gd1—O3	72.58 (7)
C6—C8—H8	119.6	O1^iv—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)	O1^iv—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—C12^iii	120.8 (2)	O3—Gd1—O1	110.02 (6)
C10—C11—H11	119.6	O7—Gd1—C9	100.03 (8)
C12^iii—C11—H11	119.6	O1W—Gd1—C9	147.76 (8)
C11^iii—C12—C10	119.4 (2)	O4—Gd1—C9	79.48 (7)
C11^iii—C12—H12	120.3	O2—Gd1—C9	100.94 (8)
C10—C12—H12	120.3	O1^iv—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	O1^iv—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—Gd1^iv	152.36 (16)	O1^iv—Gd1—C1	90.86 (6)
C1—O1—Gd1	87.44 (14)	O6—Gd1—C1	125.76 (6)
Gd1^iv—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)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—HW11···O3^v	0.73 (3)	2.10 (3)	2.832 (3)	173 (3)
O1W—HW12···O5^iv	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.