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In the title complex, [Sm(C7H3O4)(C7H4O4)(H2O)2]·4H2O, the coordination number of the Sm atom is nine. The pyridine-2,6-di­carboxyl­ate ligand chelates to the Sm atom and bridges to the neighbouring Sm atoms to form infinite chains along the c axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805012894/ob6508sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805012894/ob6508Isup2.hkl
Contains datablock I

CCDC reference: 274599

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.012 Å
  • R factor = 0.062
  • wR factor = 0.156
  • Data-to-parameter ratio = 13.7

checkCIF/PLATON results

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Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 12
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 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

catena-Poly[[[diaqua(6-carboxypyridine-2-carboxylato- κ3N,O,O')samarium(III)]-µ-pyridine-2,6-dicarboxylato-κ4N,O,O':O''] tetrahydrate] top
Crystal data top
C14H11N2O10Sm·4H2OF(000) = 1164
Mr = 589.66Dx = 1.996 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 935 reflections
a = 13.973 (3) Åθ = 2.4–25.6°
b = 11.203 (2) ŵ = 3.07 mm1
c = 12.830 (3) ÅT = 293 K
β = 102.367 (4)°Prism, colourless
V = 1961.8 (7) Å30.20 × 0.14 × 0.12 mm
Z = 4
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
3846 independent reflections
Radiation source: sealed tube2849 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.044
φ and ω scansθmax = 26.0°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1617
Tmin = 0.61, Tmax = 0.69k = 1313
10285 measured reflectionsl = 1315
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)] = 0.062Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.156H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.09P)2 + 1.99P]
where P = (Fo2 + 2Fc2)/3
3846 reflections(Δ/σ)max < 0.001
280 parametersΔρmax = 0.98 e Å3
0 restraintsΔρmin = 2.01 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.

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
xyzUiso*/Ueq
Sm10.73035 (3)0.79558 (4)0.35103 (4)0.03115 (18)
C10.5056 (7)0.6854 (8)0.3672 (7)0.0332 (19)
C20.4052 (6)0.6802 (7)0.3677 (7)0.0295 (18)
H20.37510.60670.37130.035*
C30.3525 (7)0.7811 (8)0.3627 (7)0.0332 (19)
H30.28550.77800.35970.040*
C40.4007 (6)0.8927 (8)0.3622 (7)0.0329 (19)
H40.36620.96400.35950.040*
C50.4993 (7)0.8923 (7)0.3658 (7)0.0308 (18)
C60.5576 (6)1.0028 (8)0.3650 (7)0.0317 (19)
C70.5712 (6)0.5792 (7)0.3729 (7)0.0284 (18)
C80.8718 (6)1.0350 (7)0.4407 (7)0.0289 (18)
C90.9068 (6)1.1357 (8)0.5012 (7)0.0317 (19)
H90.93261.19980.47020.038*
C100.9023 (6)1.1386 (8)0.6083 (7)0.0321 (19)
H100.92681.20360.65060.038*
C110.8614 (6)1.0443 (8)0.6504 (7)0.0336 (19)
H110.85801.04390.72200.040*
C120.8254 (7)0.9501 (8)0.5850 (7)0.0327 (19)
C130.8788 (6)1.0229 (8)0.3263 (7)0.0315 (18)
C140.7746 (6)0.8452 (7)0.6197 (6)0.0251 (16)
N10.5511 (5)0.7895 (6)0.3667 (6)0.0322 (16)
N20.8310 (5)0.9439 (6)0.4787 (6)0.0341 (17)
O10.6451 (5)0.9935 (5)0.3632 (5)0.0354 (14)
O20.5164 (5)1.0995 (5)0.3743 (5)0.0330 (14)
H2A0.47411.12010.30740.049*
O30.6583 (4)0.6014 (5)0.3678 (5)0.0322 (13)
O40.5325 (4)0.4797 (5)0.3757 (5)0.0322 (13)
O50.7810 (4)0.8300 (5)0.7164 (5)0.0312 (13)
O60.7265 (4)0.7774 (5)0.5461 (5)0.0301 (13)
O70.8438 (4)0.9274 (5)0.2805 (5)0.0300 (13)
O80.9176 (4)1.1023 (5)0.2823 (5)0.0336 (14)
O90.8731 (4)0.6867 (5)0.4348 (5)0.0273 (13)
H9A0.85410.61430.46500.041*
H9C0.91090.66750.38280.041*
O100.6330 (4)0.8453 (5)0.1765 (4)0.0305 (13)
H10A0.67090.85750.13380.037*
H10C0.60000.90810.18110.037*
O110.9600 (4)0.8069 (5)0.1489 (5)0.0312 (13)
H11D0.93720.73660.14940.037*
H11B0.91860.84540.17570.037*
O120.8020 (4)0.4057 (5)0.4116 (5)0.0316 (13)
H12A0.81580.42410.47730.038*
H12B0.74020.39990.39050.038*
O130.6293 (4)0.2760 (5)0.3857 (5)0.0340 (14)
H13A0.63270.22820.43790.041*
H13B0.58150.32350.38340.041*
O140.9710 (4)0.0574 (5)0.0974 (5)0.0303 (13)
H14B0.95460.07560.16400.036*
H14C0.98450.01630.09000.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm10.0326 (3)0.0317 (3)0.0292 (3)0.0011 (2)0.00667 (17)0.00449 (19)
C10.037 (5)0.034 (5)0.029 (5)0.002 (4)0.007 (4)0.010 (4)
C20.031 (4)0.027 (4)0.037 (5)0.004 (3)0.020 (4)0.005 (4)
C30.037 (5)0.034 (5)0.029 (4)0.002 (4)0.007 (4)0.010 (4)
C40.029 (4)0.028 (4)0.043 (5)0.008 (4)0.011 (4)0.002 (4)
C50.040 (5)0.025 (4)0.030 (5)0.015 (4)0.012 (4)0.006 (3)
C60.030 (5)0.033 (5)0.034 (5)0.010 (4)0.014 (4)0.001 (4)
C70.028 (4)0.026 (4)0.032 (4)0.003 (3)0.006 (3)0.006 (3)
C80.032 (4)0.025 (4)0.031 (5)0.006 (3)0.011 (3)0.007 (3)
C90.030 (4)0.033 (5)0.034 (5)0.010 (4)0.014 (4)0.001 (4)
C100.035 (5)0.026 (4)0.032 (5)0.010 (4)0.002 (4)0.002 (4)
C110.032 (4)0.035 (5)0.032 (5)0.007 (4)0.002 (4)0.003 (4)
C120.037 (5)0.034 (4)0.027 (4)0.004 (4)0.006 (4)0.003 (4)
C130.028 (4)0.035 (5)0.032 (5)0.007 (4)0.007 (3)0.007 (4)
C140.031 (4)0.020 (4)0.024 (4)0.002 (3)0.006 (3)0.002 (3)
N10.034 (4)0.029 (4)0.032 (4)0.004 (3)0.004 (3)0.000 (3)
N20.038 (4)0.033 (4)0.033 (4)0.013 (3)0.012 (3)0.003 (3)
O10.038 (4)0.029 (3)0.042 (4)0.001 (3)0.015 (3)0.004 (3)
O20.043 (3)0.030 (3)0.027 (3)0.016 (3)0.011 (3)0.006 (3)
O30.034 (3)0.029 (3)0.032 (3)0.004 (3)0.004 (3)0.000 (3)
O40.030 (3)0.031 (3)0.034 (3)0.006 (3)0.005 (3)0.005 (3)
O50.035 (3)0.028 (3)0.028 (3)0.007 (2)0.002 (2)0.004 (2)
O60.035 (3)0.027 (3)0.030 (3)0.002 (2)0.010 (3)0.007 (2)
O70.031 (3)0.030 (3)0.032 (3)0.008 (2)0.015 (2)0.011 (3)
O80.038 (3)0.033 (3)0.027 (3)0.013 (3)0.002 (3)0.003 (3)
O90.029 (3)0.029 (3)0.029 (3)0.009 (2)0.017 (2)0.008 (2)
O100.035 (3)0.028 (3)0.027 (3)0.015 (3)0.001 (2)0.005 (2)
O110.032 (3)0.028 (3)0.034 (3)0.001 (2)0.009 (3)0.003 (2)
O120.034 (3)0.031 (3)0.032 (3)0.001 (3)0.012 (3)0.000 (3)
O130.037 (3)0.033 (3)0.039 (4)0.007 (3)0.023 (3)0.007 (3)
O140.031 (3)0.029 (3)0.034 (3)0.010 (2)0.012 (2)0.001 (3)
Geometric parameters (Å, º) top
Sm1—O92.388 (5)C9—C101.389 (12)
Sm1—O102.423 (6)C9—H90.9300
Sm1—O32.426 (6)C10—C111.366 (13)
Sm1—O5i2.446 (6)C10—H100.9300
Sm1—O72.476 (6)C11—C121.374 (12)
Sm1—O62.524 (6)C11—H110.9300
Sm1—N22.537 (8)C12—N21.385 (11)
Sm1—O12.537 (6)C12—C141.489 (12)
Sm1—N12.556 (7)C13—O81.240 (11)
C1—N11.330 (11)C13—O71.267 (11)
C1—C21.406 (12)C14—O51.237 (10)
C1—C71.493 (12)C14—O61.283 (10)
C2—C31.343 (12)O2—H2A0.9600
C2—H20.9300O5—Sm1ii2.446 (6)
C3—C41.421 (12)O9—H9A0.9601
C3—H30.9300O9—H9C0.9600
C4—C51.369 (12)O10—H10A0.8501
C4—H40.9300O10—H10C0.8500
C5—N11.359 (11)O11—H11D0.8500
C5—C61.483 (11)O11—H11B0.8500
C6—O11.231 (10)O12—H12A0.8500
C6—O21.244 (11)O12—H12B0.8501
C7—O41.243 (10)O13—H13A0.8500
C7—O31.257 (10)O13—H13B0.8499
C8—N21.312 (11)O14—H14B0.9539
C8—C91.397 (12)O14—H14C0.8566
C8—C131.498 (12)
O9—Sm1—O10141.5 (2)C4—C5—C6123.2 (8)
O9—Sm1—O379.90 (19)O1—C6—O2123.9 (8)
O10—Sm1—O397.26 (19)O1—C6—C5118.6 (8)
O9—Sm1—O5i71.6 (2)O2—C6—C5117.3 (8)
O10—Sm1—O5i70.7 (2)O4—C7—O3127.6 (8)
O3—Sm1—O5i74.65 (19)O4—C7—C1116.7 (7)
O9—Sm1—O786.04 (18)O3—C7—C1115.5 (7)
O10—Sm1—O778.56 (19)N2—C8—C9123.4 (8)
O3—Sm1—O7151.38 (19)N2—C8—C13114.7 (8)
O5i—Sm1—O777.3 (2)C9—C8—C13121.9 (7)
O9—Sm1—O672.88 (19)C10—C9—C8118.9 (8)
O10—Sm1—O6143.9 (2)C10—C9—H9120.6
O3—Sm1—O675.08 (19)C8—C9—H9120.6
O5i—Sm1—O6136.45 (19)C11—C10—C9119.0 (8)
O7—Sm1—O6124.2 (2)C11—C10—H10120.5
O9—Sm1—N275.5 (2)C9—C10—H10120.5
O10—Sm1—N2124.8 (2)C10—C11—C12118.8 (8)
O3—Sm1—N2135.5 (2)C10—C11—H11120.6
O5i—Sm1—N2128.9 (2)C12—C11—H11120.6
O7—Sm1—N262.3 (2)C11—C12—N2123.3 (8)
O6—Sm1—N262.5 (2)C11—C12—C14124.0 (8)
O9—Sm1—O1141.0 (2)N2—C12—C14112.7 (7)
O10—Sm1—O171.2 (2)O8—C13—O7123.9 (8)
O3—Sm1—O1124.7 (2)O8—C13—C8120.5 (8)
O5i—Sm1—O1139.1 (2)O7—C13—C8115.6 (8)
O7—Sm1—O181.21 (18)O5—C14—O6124.8 (7)
O6—Sm1—O184.23 (19)O5—C14—C12118.1 (7)
N2—Sm1—O165.8 (2)O6—C14—C12117.1 (7)
O9—Sm1—N1133.5 (2)C1—N1—C5119.3 (7)
O10—Sm1—N173.3 (2)C1—N1—Sm1120.1 (6)
O3—Sm1—N162.4 (2)C5—N1—Sm1120.4 (5)
O5i—Sm1—N1118.5 (2)C8—N2—C12116.6 (8)
O7—Sm1—N1139.4 (2)C8—N2—Sm1119.6 (6)
O6—Sm1—N172.0 (2)C12—N2—Sm1121.9 (6)
N2—Sm1—N1112.5 (2)C6—O1—Sm1123.8 (5)
O1—Sm1—N162.4 (2)C6—O2—H2A109.5
N1—C1—C2121.0 (8)C7—O3—Sm1127.3 (5)
N1—C1—C7114.2 (8)C14—O5—Sm1ii144.9 (5)
C2—C1—C7124.7 (7)C14—O6—Sm1124.2 (5)
C3—C2—C1120.1 (8)C13—O7—Sm1123.2 (5)
C3—C2—H2119.9Sm1—O9—H9A109.7
C1—C2—H2119.9Sm1—O9—H9C109.4
C2—C3—C4119.1 (8)H9A—O9—H9C109.5
C2—C3—H3120.5Sm1—O10—H10A109.2
C4—C3—H3120.5Sm1—O10—H10C109.4
C5—C4—C3118.2 (8)H10A—O10—H10C109.5
C5—C4—H4120.9H11D—O11—H11B100.3
C3—C4—H4120.9H12A—O12—H12B109.5
N1—C5—C4122.2 (7)H13A—O13—H13B109.5
N1—C5—C6114.5 (8)H14B—O14—H14C113.9
Symmetry codes: (i) x, y+3/2, z1/2; (ii) x, y+3/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H2A···O3iii0.962.603.515 (9)161
O9—H9A···O120.962.503.295 (8)140
O9—H9C···O14iv0.962.032.720 (7)127
O10—H10A···O6i0.852.132.707 (8)125
O10—H10C···O10.852.482.889 (8)111
O10—H10C···O4iii0.852.012.720 (9)141
O11—H11B···O70.852.082.912 (8)164
O12—H12A···O14v0.852.393.004 (9)130
O12—H12B···O30.852.522.945 (8)112
O12—H12B···O130.852.072.775 (8)140
O13—H13B···O40.851.872.642 (8)150
O14—H14B···O8vi0.951.732.683 (8)176
O14—H14C···O11vi0.862.172.895 (8)142
Symmetry codes: (i) x, y+3/2, z1/2; (iii) x+1, y+1/2, z+1/2; (iv) x+2, y+1/2, z+1/2; (v) x, y+1/2, z+1/2; (vi) x, y1, z.
 

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