Retracted: catena-Poly[[[diaqua­(6-carboxypyridine-2-carboxyl­ato)­samarium(II)]-μ-pyridine-2,6-dicarboxyl­ato] tetra­hydrate]

The title compound, {[Sm(C₇H₃NO₄)(C₇H₄NO₄)(H₂O)₂]·4H₂O}_n, is isostructural with its La^III, Ce^III, Pr^III and Nd^III analogues and has been prepared by a hydro­thermal reaction of samarium(III) nitrate (hydrate)_n and pyridine-2,6-dicarboxylic acid. The asymmetric unit contains one Sm^III ion, two pyridine-2,6-dicarboxyl­ate anions (one of them only singly deprotonated), and six water molecules. The Sm^III atoms are linked via bridging pyridine-2,6-dicarboxyl­ate ligands, yielding a chain structure.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.032
• wR factor = 0.095
• Data-to-parameter ratio = 11.2

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT220_ALERT_2_B Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       4.30 Ratio
PLAT420_ALERT_2_B D-H Without Acceptor       O104   -   H4C    ...          ?

Alert level C
SHFSU01_ALERT_2_C  The absolute value of parameter shift to su ratio > 0.05
            Absolute value of the parameter shift to su ratio given   0.100
            Additional refinement cycles may be required.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT080_ALERT_2_C Maximum Shift/Error ............................       0.10
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       2.51 Ratio
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.15 Ratio
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         C4
PLAT245_ALERT_2_C U(iso) H1C     Smaller than U(eq) O101    by ...       0.01 AngSq
PLAT245_ALERT_2_C U(iso) H1D     Smaller than U(eq) O101    by ...       0.01 AngSq
PLAT245_ALERT_2_C U(iso) H4C     Smaller than U(eq) O104    by ...       0.01 AngSq
PLAT245_ALERT_2_C U(iso) H4D     Smaller than U(eq) O104    by ...       0.01 AngSq
PLAT731_ALERT_1_C Bond    Calc     0.90(7), Rep     0.90(3) ......       2.33 su-Ra
              O1   -H7C     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.88(7), Rep     0.88(3) ......       2.33 su-Ra
              O9   -H9B     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.82(7), Rep     0.82(3) ......       2.33 su-Ra
              O10  -H10C    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(7), Rep     0.85(3) ......       2.33 su-Ra
              O103 -H3C     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.86(7), Rep     0.86(3) ......       2.33 su-Ra
              O103 -H3D     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.82(7), Rep     0.82(3) ......       2.33 su-Ra
              O10  -H10C    1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.90(7), Rep     0.90(3) ......       2.33 su-Ra
              O1   -H7C     1.555   1.555

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
  17 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

  10 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  10 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
   0 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

---

Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT and SHELXTL (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

catena-Poly[[[diaqua(pyridine-2,6-dicarboxylato)samarium(II)]-µ-pyridine- 2,6-dicarboxylato] tetrahydrate]

Crystal data

[Sm(C7H3NO4)(C7H4NO4)(H2O)2]·4H2O	F(000) = 1164
Mr = 589.66	Dx = 1.950 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 3496 reflections
a = 14.1140 (3) Å	θ = 1.5–25.0°
b = 11.2266 (2) Å	µ = 3.00 mm^−1
c = 12.9548 (2) Å	T = 293 K
β = 101.931 (1)°	Block, purple
V = 2008.37 (6) Å^3	0.35 × 0.35 × 0.35 mm
Z = 4

Data collection

Bruker SMART CCD area-detector diffractometer	3235 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.022
Graphite monochromator	θmax = 25.0°, θmin = 1.5°
φ and ω scans	h = −16→16
7165 measured reflections	k = −13→13
3496 independent reflections	l = −7→15

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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.095	H atoms treated by a mixture of independent and constrained refinement
S = 1.00	w = 1/[σ^2(Fo^2) + (0.0635P)^2 + 7.0228P] where P = (Fo^2 + 2Fc^2)/3
3496 reflections	(Δ/σ)max = 0.100
313 parameters	Δρmax = 0.92 e Å^−3
18 restraints	Δρmin = −1.14 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
Sm1	0.230156 (16)	0.794804 (19)	0.851563 (16)	0.01742 (12)
C1	0.0578 (4)	0.9997 (5)	0.8683 (4)	0.0326 (12)
C2	−0.0026 (4)	0.8901 (5)	0.8669 (4)	0.0332 (12)
C3	−0.1017 (5)	0.8897 (7)	0.8637 (6)	0.0547 (18)
H3A	−0.1359	0.9607	0.8618	0.066*
C4	−0.1476 (6)	0.7826 (7)	0.8634 (9)	0.071 (3)
H4A	−0.2140	0.7800	0.8604	0.085*
C5	−0.0953 (5)	0.6786 (7)	0.8677 (7)	0.0540 (18)
H5A	−0.1254	0.6051	0.8692	0.065*
C6	0.0029 (4)	0.6852 (5)	0.8696 (4)	0.0298 (11)
C7	0.0678 (4)	0.5771 (5)	0.8726 (4)	0.0270 (11)
C8	0.2744 (3)	0.8471 (4)	1.1192 (3)	0.0173 (9)
C9	0.3263 (3)	0.9520 (4)	1.0831 (3)	0.0170 (9)
C10	0.3622 (3)	1.0468 (4)	1.1488 (3)	0.0224 (10)
H10A	0.3594	1.0459	1.2199	0.027*
C11	0.4016 (4)	1.1411 (4)	1.1062 (4)	0.0280 (11)
H11A	0.4240	1.2068	1.1479	0.034*
C12	0.4085 (4)	1.1393 (4)	1.0006 (4)	0.0252 (10)
H12A	0.4356	1.2028	0.9708	0.030*
C13	0.3732 (3)	1.0391 (4)	0.9407 (3)	0.0165 (9)
C14	0.3805 (3)	1.0248 (4)	0.8264 (4)	0.0217 (10)
N1	0.0479 (3)	0.7884 (3)	0.8677 (3)	0.0241 (9)
N2	0.3316 (3)	0.9486 (3)	0.9814 (3)	0.0147 (7)
O1	0.0126 (4)	1.0995 (4)	0.8736 (4)	0.0526 (12)
O2	0.1433 (3)	0.9921 (3)	0.8651 (3)	0.0294 (8)
O3	0.0306 (3)	0.4780 (4)	0.8765 (4)	0.0451 (11)
O4	0.1558 (2)	0.5971 (3)	0.8704 (3)	0.0272 (8)
O5	0.2813 (2)	0.8335 (3)	1.2162 (2)	0.0235 (7)
O6	0.2270 (3)	0.7815 (3)	1.0471 (2)	0.0210 (7)
O7	0.4207 (3)	1.1046 (3)	0.7852 (3)	0.0335 (9)
O8	0.3450 (3)	0.9294 (3)	0.7820 (2)	0.0261 (8)
O9	0.3751 (3)	0.6840 (3)	0.9368 (3)	0.0301 (8)
H9A	0.3877	0.6990	1.0001	0.045*
O10	0.1334 (3)	0.8450 (4)	0.6739 (3)	0.0415 (11)
H10B	0.0870	0.8863	0.6802	0.062*
O101	0.1237 (5)	0.2735 (5)	0.8836 (7)	0.091 (2)
O102	0.5299 (3)	0.5577 (4)	0.9015 (3)	0.0382 (9)
O103	0.4582 (3)	0.6920 (3)	0.1490 (3)	0.0293 (8)
O104	0.2978 (5)	0.4026 (5)	0.9154 (6)	0.092 (2)
H10C	0.158 (6)	0.832 (8)	0.623 (5)	0.080*
H1D	0.185 (3)	0.246 (7)	0.902 (7)	0.080*
H3C	0.428 (6)	0.677 (7)	0.198 (5)	0.080*
H9B	0.419 (5)	0.637 (6)	0.919 (5)	0.080*
H3D	0.497 (5)	0.751 (6)	0.167 (6)	0.080*
H2C	0.541 (6)	0.575 (6)	0.840 (4)	0.080*
H2D	0.527 (6)	0.480 (3)	0.902 (6)	0.080*
H4C	0.284 (6)	0.404 (8)	0.984 (4)	0.080*
H4D	0.358 (3)	0.425 (8)	0.933 (6)	0.080*
H1C	0.123 (6)	0.347 (3)	0.902 (7)	0.080*
H7C	0.042 (6)	1.168 (5)	0.863 (7)	0.080*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sm1	0.01863 (17)	0.01842 (17)	0.01454 (16)	−0.00108 (8)	0.00191 (10)	−0.00125 (8)
C1	0.040 (3)	0.025 (3)	0.031 (3)	0.010 (2)	0.004 (2)	−0.003 (2)
C2	0.029 (3)	0.036 (3)	0.035 (3)	0.013 (2)	0.007 (2)	−0.002 (2)
C3	0.032 (3)	0.056 (4)	0.079 (5)	0.019 (3)	0.019 (3)	0.006 (4)
C4	0.029 (4)	0.065 (5)	0.123 (8)	0.006 (3)	0.027 (4)	0.008 (5)
C5	0.027 (3)	0.051 (4)	0.087 (6)	0.000 (3)	0.020 (3)	0.011 (4)
C6	0.021 (3)	0.034 (3)	0.034 (3)	0.001 (2)	0.004 (2)	0.001 (2)
C7	0.020 (3)	0.031 (3)	0.029 (3)	−0.002 (2)	0.002 (2)	0.000 (2)
C8	0.019 (2)	0.019 (2)	0.015 (2)	−0.0013 (18)	0.0032 (17)	0.0018 (17)
C9	0.018 (2)	0.018 (2)	0.014 (2)	0.0026 (17)	0.0017 (17)	0.0014 (17)
C10	0.029 (3)	0.023 (2)	0.014 (2)	−0.004 (2)	0.0013 (18)	−0.0016 (18)
C11	0.036 (3)	0.024 (3)	0.021 (2)	−0.008 (2)	0.000 (2)	−0.0058 (19)
C12	0.032 (3)	0.020 (2)	0.025 (2)	−0.007 (2)	0.008 (2)	−0.0017 (19)
C13	0.016 (2)	0.015 (2)	0.018 (2)	−0.0013 (17)	0.0027 (16)	0.0005 (17)
C14	0.023 (2)	0.024 (2)	0.019 (2)	−0.0020 (19)	0.0049 (18)	0.0005 (19)
N1	0.021 (2)	0.029 (2)	0.022 (2)	0.0006 (16)	0.0024 (17)	0.0002 (16)
N2	0.0152 (18)	0.0155 (18)	0.0130 (17)	−0.0019 (14)	0.0020 (13)	−0.0012 (14)
O1	0.055 (3)	0.031 (2)	0.071 (3)	0.017 (2)	0.010 (2)	−0.004 (2)
O2	0.029 (2)	0.0202 (17)	0.037 (2)	0.0076 (15)	0.0015 (15)	−0.0028 (15)
O3	0.034 (2)	0.026 (2)	0.073 (3)	−0.0118 (17)	0.005 (2)	0.003 (2)
O4	0.0260 (19)	0.0192 (17)	0.0356 (19)	−0.0018 (14)	0.0048 (15)	−0.0018 (14)
O5	0.0319 (19)	0.0233 (17)	0.0140 (16)	−0.0081 (15)	0.0019 (14)	0.0014 (13)
O6	0.0262 (18)	0.0229 (17)	0.0135 (15)	−0.0105 (13)	0.0032 (13)	−0.0009 (12)
O7	0.054 (2)	0.0262 (18)	0.0254 (18)	−0.0160 (17)	0.0186 (17)	0.0006 (15)
O8	0.040 (2)	0.0237 (17)	0.0167 (16)	−0.0128 (15)	0.0108 (14)	−0.0043 (13)
O9	0.030 (2)	0.042 (2)	0.0167 (17)	0.0126 (16)	−0.0003 (15)	−0.0061 (15)
O10	0.045 (2)	0.061 (3)	0.0170 (18)	0.034 (2)	0.0011 (16)	0.0003 (18)
O101	0.073 (4)	0.041 (3)	0.154 (7)	0.001 (3)	0.009 (5)	−0.006 (4)
O102	0.052 (3)	0.034 (2)	0.034 (2)	0.0118 (19)	0.0238 (19)	0.0023 (17)
O103	0.031 (2)	0.033 (2)	0.0230 (19)	−0.0026 (15)	0.0046 (16)	0.0001 (15)
O104	0.067 (4)	0.046 (3)	0.147 (6)	0.012 (3)	−0.013 (4)	−0.007 (4)

Geometric parameters (Å, º)

Sm1—O9	2.454 (4)	C9—N2	1.336 (5)
Sm1—O10	2.486 (3)	C9—C10	1.391 (6)
Sm1—O5^i	2.489 (3)	C10—C11	1.365 (7)
Sm1—O4	2.489 (3)	C10—H10A	0.9300
Sm1—O8	2.515 (3)	C11—C12	1.392 (7)
Sm1—O6	2.548 (3)	C11—H11A	0.9300
Sm1—O2	2.556 (3)	C12—C13	1.398 (6)
Sm1—N2	2.620 (3)	C12—H12A	0.9300
Sm1—N1	2.625 (4)	C13—N2	1.335 (6)
C1—O2	1.218 (7)	C13—C14	1.515 (6)
C1—O1	1.298 (7)	C14—O7	1.240 (6)
C1—C2	1.496 (8)	C14—O8	1.268 (6)
C2—N1	1.344 (7)	O1—H7C	0.90 (3)
C2—C3	1.390 (8)	O5—Sm1^ii	2.489 (3)
C3—C4	1.365 (11)	O9—H9A	0.8200
C3—H3A	0.9300	O9—H9B	0.88 (3)
C4—C5	1.377 (10)	O10—H10B	0.8200
C4—H4A	0.9300	O10—H10C	0.82 (3)
C5—C6	1.382 (8)	O101—H1D	0.90 (3)
C5—H5A	0.9300	O101—H1C	0.86 (3)
C6—N1	1.324 (7)	O102—H2C	0.87 (3)
C6—C7	1.517 (7)	O102—H2D	0.87 (3)
C7—O3	1.235 (6)	O103—H3C	0.85 (3)
C7—O4	1.268 (6)	O103—H3D	0.86 (3)
C8—O5	1.250 (5)	O104—H4C	0.94 (3)
C8—O6	1.266 (6)	O104—H4D	0.87 (3)
C8—C9	1.510 (6)
O9—Sm1—O10	141.19 (12)	C6—C5—H5A	120.6
O9—Sm1—O5^i	71.78 (11)	N1—C6—C5	122.0 (6)
O10—Sm1—O5^i	70.30 (11)	N1—C6—C7	114.3 (5)
O9—Sm1—O4	80.37 (13)	C5—C6—C7	123.8 (5)
O10—Sm1—O4	97.53 (14)	O3—C7—O4	125.9 (5)
O5^i—Sm1—O4	75.09 (11)	O3—C7—C6	117.5 (5)
O9—Sm1—O8	85.80 (13)	O4—C7—C6	116.6 (4)
O10—Sm1—O8	78.68 (14)	O5—C8—O6	126.1 (4)
O5^i—Sm1—O8	78.04 (11)	O5—C8—C9	117.7 (4)
O4—Sm1—O8	152.49 (11)	O6—C8—C9	116.2 (4)
O9—Sm1—O6	72.96 (12)	N2—C9—C10	122.5 (4)
O10—Sm1—O6	144.55 (12)	N2—C9—C8	114.4 (4)
O5^i—Sm1—O6	137.23 (11)	C10—C9—C8	123.1 (4)
O4—Sm1—O6	75.85 (11)	C11—C10—C9	118.3 (4)
O8—Sm1—O6	122.45 (10)	C11—C10—H10A	120.9
O9—Sm1—O2	140.90 (12)	C9—C10—H10A	120.9
O10—Sm1—O2	71.77 (12)	C10—C11—C12	120.2 (4)
O5^i—Sm1—O2	139.75 (11)	C10—C11—H11A	119.9
O4—Sm1—O2	123.25 (12)	C12—C11—H11A	119.9
O8—Sm1—O2	81.83 (12)	C11—C12—C13	117.9 (4)
O6—Sm1—O2	82.83 (11)	C11—C12—H12A	121.0
O9—Sm1—N2	75.57 (12)	C13—C12—H12A	121.0
O10—Sm1—N2	124.58 (14)	N2—C13—C12	121.9 (4)
O5^i—Sm1—N2	129.33 (11)	N2—C13—C14	115.4 (4)
O4—Sm1—N2	135.26 (11)	C12—C13—C14	122.7 (4)
O8—Sm1—N2	61.76 (10)	O7—C14—O8	126.1 (4)
O6—Sm1—N2	61.31 (10)	O7—C14—C13	118.3 (4)
O2—Sm1—N2	65.87 (11)	O8—C14—C13	115.6 (4)
O9—Sm1—N1	133.64 (13)	C6—N1—C2	119.2 (5)
O10—Sm1—N1	73.73 (14)	C6—N1—Sm1	120.5 (3)
O5^i—Sm1—N1	118.18 (12)	C2—N1—Sm1	120.2 (3)
O4—Sm1—N1	61.83 (12)	C13—N2—C9	119.1 (4)
O8—Sm1—N1	139.44 (12)	C13—N2—Sm1	118.4 (3)
O6—Sm1—N1	72.56 (12)	C9—N2—Sm1	121.1 (3)
O2—Sm1—N1	61.70 (12)	C1—O1—H7C	119 (6)
N2—Sm1—N1	112.44 (12)	C1—O2—Sm1	123.8 (3)
O2—C1—O1	124.3 (5)	C7—O4—Sm1	126.5 (3)
O2—C1—C2	120.5 (5)	C8—O5—Sm1^ii	143.7 (3)
O1—C1—C2	115.2 (5)	C8—O6—Sm1	125.7 (3)
N1—C2—C3	121.7 (6)	C14—O8—Sm1	124.6 (3)
N1—C2—C1	113.5 (4)	Sm1—O9—H9A	109.5
C3—C2—C1	124.8 (5)	Sm1—O9—H9B	139 (4)
C4—C3—C2	118.5 (6)	H9A—O9—H9B	111.6
C4—C3—H3A	120.8	Sm1—O10—H10B	109.5
C2—C3—H3A	120.8	Sm1—O10—H10C	118 (6)
C3—C4—C5	119.7 (7)	H10B—O10—H10C	131.2
C3—C4—H4A	120.1	H1D—O101—H1C	109 (6)
C5—C4—H4A	120.1	H2C—O102—H2D	105 (5)
C4—C5—C6	118.9 (7)	H3C—O103—H3D	111 (6)
C4—C5—H5A	120.6	H4C—O104—H4D	98 (5)

Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x, −y+3/2, z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O9—H9A···O103^iii	0.82	1.98	2.758 (5)	158
O10—H10B···O3^iv	0.82	1.96	2.719 (5)	153
O10—H10C···O6^i	0.82 (3)	1.98 (5)	2.712 (5)	147 (8)
O102—H2C···O7^v	0.87 (3)	1.84 (3)	2.704 (5)	173 (8)
O102—H2D···O103^vi	0.87 (3)	2.07 (4)	2.892 (5)	157 (7)
O1—H7C···O101^vii	0.90 (3)	1.64 (5)	2.492 (8)	158 (9)

Symmetry codes: (i) x, −y+3/2, z−1/2; (iii) x, y, z+1; (iv) −x, y+1/2, −z+3/2; (v) −x+1, y−1/2, −z+3/2; (vi) −x+1, −y+1, −z+1; (vii) x, y+1, z.