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The title complex, [Dy2(C7H3NO4)3(H2O)3]n, contains two independent dysprosium centers which are connected through two carboxylate O atoms into a binuclear unit. Each binuclear unit is linked to symmetry-related units by four 4-pyridine-3,5-dicarboxyl­ate ligands to form a two-dimensional layer structure parallel to the ac plane. These two-dimensional layers are, in turn, linked into a three-dimensional network via shared carboxyl­ate O atoms.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806051622/lh2235sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806051622/lh2235Isup2.hkl
Contains datablock I

CCDC reference: 633909

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • Mean [sigma](C-C) = 0.009 Å
  • H-atom completeness 61%
  • R factor = 0.036
  • wR factor = 0.110
  • Data-to-parameter ratio = 11.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 100 Deg. PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 4 PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.52 Ratio PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.06 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.13 Ratio
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C21 H15 Dy2 N3 O15 Atom count from the _atom_site data: C21 H9 Dy2 N3 O15 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C21 H15 Dy2 N3 O15 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 42.00 42.00 0.00 H 30.00 18.00 12.00 Dy 4.00 4.00 0.00 N 6.00 6.00 0.00 O 30.00 30.00 0.00
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2004); software used to prepare material for publication: SHELXTL.

Poly[triaquatris(µ-4-pyridine-3,5-dicarboxylato)didysprosium(III)] top
Crystal data top
[Dy2(C7H3NO4)3(H2O)3]Z = 2
Mr = 874.36F(000) = 828
Triclinic, P1Dx = 2.488 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.9266 (2) ÅCell parameters from 6372 reflections
b = 9.3595 (1) Åθ = 1.4–25.7°
c = 14.722 (3) ŵ = 6.44 mm1
α = 97.781 (1)°T = 273 K
β = 95.518 (1)°Needle, colorless
γ = 104.819 (1)°0.10 × 0.05 × 0.03 mm
V = 1167.1 (2) Å3
Data collection top
Bruker SMART CCD
diffractometer
4351 independent reflections
Radiation source: fine-focus sealed tube4055 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
Detector resolution: 14.6306 pixels mm-1θmax = 25.7°, θmin = 1.4°
ω scansh = 107
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1111
Tmin = 0.672, Tmax = 0.826l = 1717
6372 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)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.110H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0721P)2 + 10.4697P]
where P = (Fo2 + 2Fc2)/3
4351 reflections(Δ/σ)max < 0.001
370 parametersΔρmax = 1.24 e Å3
24 restraintsΔρmin = 2.03 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
Dy10.14045 (3)0.26704 (3)0.27409 (2)0.01651 (12)
O10.0066 (5)0.6215 (5)0.1769 (3)0.0168 (9)
N10.1047 (6)0.2349 (6)0.0635 (4)0.0147 (10)
C10.1193 (7)0.5877 (6)0.1378 (4)0.0091 (11)
Dy20.54192 (3)0.14825 (3)0.16656 (2)0.01801 (12)
O20.2603 (5)0.6631 (5)0.1282 (3)0.0169 (9)
N20.4848 (7)0.2491 (6)0.5265 (4)0.0171 (11)
C20.0861 (7)0.4471 (6)0.0950 (4)0.0085 (11)
O30.4244 (5)0.2707 (5)0.0457 (3)0.0182 (9)
N30.8898 (6)0.6687 (6)0.3242 (4)0.0201 (12)
C30.0661 (7)0.3557 (7)0.1060 (4)0.0137 (12)
H30.14360.37830.14380.016*
O40.2406 (5)0.1719 (5)0.1280 (3)0.0147 (9)
C40.0088 (7)0.2024 (7)0.0097 (4)0.0142 (12)
H40.01790.12080.02090.017*
O50.2497 (6)0.2143 (5)0.3021 (3)0.0196 (10)
C50.1643 (7)0.2860 (6)0.0017 (4)0.0094 (11)
O60.0418 (5)0.1883 (6)0.3880 (3)0.0227 (10)
C60.2037 (6)0.4101 (7)0.0415 (4)0.0104 (11)
H60.30690.46800.03500.012*
O70.2327 (5)0.0700 (5)0.6681 (3)0.0185 (9)
C70.2841 (7)0.2399 (6)0.0622 (4)0.0123 (11)
O80.4231 (6)0.0050 (6)0.7298 (3)0.0239 (10)
C80.1798 (7)0.1967 (6)0.3761 (4)0.0135 (12)
O90.4647 (5)0.3444 (5)0.2712 (3)0.0164 (9)
C90.2715 (7)0.1847 (7)0.4572 (4)0.0119 (11)
O100.3378 (5)0.5082 (5)0.2376 (4)0.0270 (12)
C100.3926 (7)0.2540 (7)0.4595 (4)0.0137 (12)
H100.41040.30640.41210.016*
O110.6978 (5)0.9808 (5)0.1403 (3)0.0159 (9)
C110.4574 (7)0.1725 (7)0.5933 (4)0.0142 (12)
H110.52020.16800.64030.017*
O120.9515 (5)1.0409 (5)0.1973 (3)0.0148 (9)
C120.3401 (7)0.0985 (6)0.5968 (4)0.0095 (11)
C130.2427 (7)0.1079 (6)0.5280 (4)0.0112 (11)
H130.16050.06380.52970.013*
C140.3310 (7)0.0034 (6)0.6713 (4)0.0126 (12)
C150.4620 (7)0.4750 (7)0.2556 (4)0.0145 (12)
C160.6168 (7)0.5910 (6)0.2623 (4)0.0109 (11)
C170.6346 (7)0.7189 (7)0.2216 (4)0.0113 (11)
H170.54940.73620.18770.014*
C180.7815 (7)0.8206 (6)0.2323 (4)0.0102 (11)
C190.9050 (7)0.7912 (7)0.2849 (4)0.0173 (13)
H191.00290.86030.29310.021*
C200.7492 (8)0.5706 (7)0.3117 (5)0.0172 (13)
H200.73860.48360.33730.021*
C210.8133 (7)0.9599 (6)0.1868 (4)0.0097 (11)
O1W0.2720 (7)0.3543 (7)0.4479 (4)0.0365 (14)
O2W0.0991 (7)0.5035 (6)0.3668 (4)0.0336 (13)
O3W0.3982 (5)0.0818 (6)0.0550 (4)0.0257 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Dy10.01234 (18)0.01591 (17)0.02269 (19)0.00379 (12)0.00071 (12)0.00937 (12)
O10.0146 (18)0.0167 (18)0.0225 (19)0.0076 (15)0.0022 (15)0.0116 (15)
N10.008 (2)0.014 (3)0.021 (3)0.000 (2)0.000 (2)0.008 (2)
C10.008 (3)0.006 (3)0.013 (3)0.000 (2)0.002 (2)0.005 (2)
Dy20.01282 (18)0.01763 (19)0.02464 (19)0.00282 (13)0.00111 (13)0.01081 (13)
O20.0133 (18)0.0155 (18)0.0212 (18)0.0010 (15)0.0007 (15)0.0121 (15)
N20.023 (3)0.019 (3)0.017 (3)0.014 (2)0.006 (2)0.010 (2)
C20.011 (3)0.008 (3)0.009 (3)0.003 (2)0.003 (2)0.006 (2)
O30.008 (2)0.028 (2)0.023 (2)0.0044 (18)0.0016 (17)0.0158 (19)
N30.013 (3)0.015 (3)0.031 (3)0.001 (2)0.007 (2)0.011 (2)
C30.006 (3)0.017 (3)0.019 (3)0.003 (2)0.002 (2)0.007 (2)
O40.011 (2)0.018 (2)0.017 (2)0.0025 (17)0.0001 (16)0.0118 (17)
C40.014 (3)0.011 (3)0.017 (3)0.000 (2)0.000 (2)0.006 (2)
O50.024 (2)0.025 (2)0.013 (2)0.009 (2)0.0052 (18)0.0094 (18)
C50.009 (3)0.010 (3)0.011 (3)0.004 (2)0.001 (2)0.004 (2)
O60.013 (2)0.034 (3)0.024 (2)0.006 (2)0.0067 (18)0.009 (2)
C60.002 (3)0.012 (3)0.016 (3)0.000 (2)0.000 (2)0.003 (2)
O70.015 (2)0.020 (2)0.025 (2)0.0090 (19)0.0016 (18)0.0157 (19)
C70.011 (3)0.010 (3)0.015 (3)0.001 (2)0.000 (2)0.005 (2)
O80.029 (3)0.028 (3)0.024 (2)0.013 (2)0.014 (2)0.019 (2)
C80.016 (3)0.010 (3)0.015 (3)0.000 (2)0.004 (2)0.007 (2)
O90.012 (2)0.012 (2)0.025 (2)0.0008 (17)0.0004 (18)0.0094 (18)
C90.009 (3)0.015 (3)0.011 (3)0.001 (2)0.002 (2)0.006 (2)
O100.008 (2)0.015 (2)0.058 (3)0.0001 (18)0.002 (2)0.014 (2)
C100.014 (3)0.012 (3)0.017 (3)0.005 (2)0.000 (2)0.009 (2)
O110.014 (2)0.012 (2)0.023 (2)0.0053 (17)0.0014 (17)0.0065 (17)
C110.015 (3)0.016 (3)0.016 (3)0.008 (2)0.005 (2)0.006 (2)
O120.007 (2)0.0083 (19)0.026 (2)0.0029 (16)0.0017 (17)0.0053 (17)
C120.010 (2)0.009 (2)0.010 (2)0.0017 (17)0.0011 (17)0.0064 (17)
C130.010 (3)0.012 (3)0.013 (3)0.005 (2)0.001 (2)0.004 (2)
C140.011 (3)0.011 (3)0.015 (3)0.002 (2)0.002 (2)0.009 (2)
C150.010 (3)0.013 (3)0.019 (3)0.004 (2)0.004 (2)0.006 (2)
C160.005 (3)0.008 (3)0.017 (3)0.003 (2)0.001 (2)0.002 (2)
C170.007 (3)0.012 (3)0.015 (3)0.004 (2)0.000 (2)0.001 (2)
C180.007 (3)0.009 (3)0.016 (3)0.002 (2)0.001 (2)0.003 (2)
C190.014 (2)0.014 (2)0.022 (2)0.0006 (19)0.0005 (19)0.0058 (19)
C200.020 (3)0.007 (3)0.026 (3)0.004 (2)0.000 (3)0.009 (2)
C210.009 (3)0.010 (3)0.013 (3)0.006 (2)0.005 (2)0.002 (2)
O1W0.035 (3)0.040 (3)0.034 (3)0.023 (3)0.019 (2)0.003 (2)
O2W0.039 (3)0.030 (3)0.034 (3)0.025 (3)0.012 (2)0.005 (2)
O3W0.010 (2)0.023 (3)0.036 (3)0.0082 (19)0.0014 (19)0.008 (2)
Geometric parameters (Å, º) top
Dy1—O1i2.367 (4)O5—C81.254 (8)
Dy1—O12ii2.400 (4)O5—Dy2vii2.488 (5)
Dy1—O7iii2.423 (4)C5—C61.383 (8)
Dy1—O62.500 (5)C5—C71.509 (8)
Dy1—O42.545 (4)O6—C81.252 (8)
Dy1—O2W2.568 (5)C6—H60.9300
Dy1—O1W2.638 (5)O7—C141.245 (8)
Dy1—O102.639 (5)O7—Dy1iii2.423 (4)
Dy1—O92.804 (4)O8—C141.248 (8)
O1—C11.243 (7)O8—Dy2iii2.374 (4)
O1—Dy1i2.367 (4)C8—C91.512 (8)
N1—C41.347 (8)O9—C151.280 (8)
N1—C31.350 (8)C9—C131.385 (8)
C1—O21.260 (7)C9—C101.396 (8)
C1—C21.509 (7)O10—C151.240 (8)
Dy2—O2iv2.328 (4)C10—H100.9300
Dy2—O11v2.365 (4)O11—C211.255 (7)
Dy2—O8iii2.374 (4)O11—Dy2viii2.365 (4)
Dy2—O5vi2.488 (5)C11—C121.396 (8)
Dy2—O3W2.490 (5)C11—H110.9300
Dy2—O92.511 (5)O12—C211.255 (7)
Dy2—O32.528 (4)O12—Dy1ix2.400 (4)
Dy2—O42.766 (4)C12—C131.394 (8)
O2—Dy2iv2.328 (4)C12—C141.512 (7)
N2—C111.333 (8)C13—H130.9300
N2—C101.342 (8)C15—C161.508 (8)
C2—C31.389 (8)C16—C171.390 (8)
C2—C61.394 (8)C16—C201.396 (8)
O3—C71.266 (8)C17—C181.390 (8)
N3—C201.331 (8)C17—H170.9300
N3—C191.334 (8)C18—C191.393 (9)
C3—H30.9300C18—C211.521 (8)
O4—C71.268 (7)C19—H190.9300
C4—C51.389 (8)C20—H200.9300
C4—H40.9300
O1i—Dy1—O12ii82.54 (15)C6—C2—C1121.4 (5)
O1i—Dy1—O7iii158.04 (16)C7—O3—Dy299.8 (4)
O12ii—Dy1—O7iii76.17 (15)C20—N3—C19117.8 (5)
O1i—Dy1—O6102.09 (15)N1—C3—C2121.8 (5)
O12ii—Dy1—O673.82 (16)N1—C3—H3119.1
O7iii—Dy1—O677.22 (16)C2—C3—H3119.1
O1i—Dy1—O485.99 (14)C7—O4—Dy1129.2 (4)
O12ii—Dy1—O471.86 (14)C7—O4—Dy288.5 (3)
O7iii—Dy1—O482.37 (14)Dy1—O4—Dy2111.28 (15)
O6—Dy1—O4143.31 (15)N1—C4—C5122.6 (5)
O1i—Dy1—O2W70.40 (16)N1—C4—H4118.7
O12ii—Dy1—O2W129.71 (17)C5—C4—H4118.7
O7iii—Dy1—O2W128.29 (17)C8—O5—Dy2vii156.0 (4)
O6—Dy1—O2W71.68 (19)C6—C5—C4118.8 (5)
O4—Dy1—O2W142.88 (17)C6—C5—C7122.2 (5)
O1i—Dy1—O1W131.15 (16)C4—C5—C7119.0 (5)
O12ii—Dy1—O1W131.70 (17)C8—O6—Dy1120.5 (4)
O7iii—Dy1—O1W69.22 (16)C5—C6—C2118.9 (5)
O6—Dy1—O1W66.56 (18)C5—C6—H6120.6
O4—Dy1—O1W132.45 (16)C2—C6—H6120.6
O2W—Dy1—O1W60.86 (16)C14—O7—Dy1iii146.2 (4)
O1i—Dy1—O1073.39 (15)O3—C7—O4122.3 (5)
O12ii—Dy1—O10140.94 (16)O3—C7—C5119.0 (5)
O7iii—Dy1—O10121.16 (15)O4—C7—C5118.7 (5)
O6—Dy1—O10140.55 (17)C14—O8—Dy2iii139.1 (4)
O4—Dy1—O1076.12 (16)O6—C8—O5125.6 (6)
O2W—Dy1—O1069.98 (19)O6—C8—C9117.8 (5)
O1W—Dy1—O1086.74 (19)O5—C8—C9116.5 (5)
O1i—Dy1—O9116.61 (14)C15—O9—Dy2126.8 (4)
O12ii—Dy1—O9127.32 (14)C15—O9—Dy190.3 (3)
O7iii—Dy1—O973.78 (14)Dy2—O9—Dy1111.11 (15)
O6—Dy1—O9136.78 (14)C13—C9—C10118.8 (5)
O4—Dy1—O962.12 (13)C13—C9—C8123.5 (5)
O2W—Dy1—O9102.81 (16)C10—C9—C8117.7 (5)
O1W—Dy1—O973.47 (16)C15—O10—Dy199.1 (4)
O10—Dy1—O947.68 (13)N2—C10—C9123.6 (5)
C1—O1—Dy1i161.0 (4)N2—C10—H10118.2
C4—N1—C3118.5 (5)C9—C10—H10118.2
O1—C1—O2125.6 (5)C21—O11—Dy2viii133.5 (4)
O1—C1—C2118.0 (5)N2—C11—C12123.8 (6)
O2—C1—C2116.3 (5)N2—C11—H11118.1
O2iv—Dy2—O11v88.94 (15)C12—C11—H11118.1
O2iv—Dy2—O8iii153.15 (17)C21—O12—Dy1ix147.7 (4)
O11v—Dy2—O8iii87.22 (16)C13—C12—C11118.5 (5)
O2iv—Dy2—O5vi75.39 (15)C13—C12—C14122.8 (5)
O11v—Dy2—O5vi73.93 (15)C11—C12—C14118.6 (5)
O8iii—Dy2—O5vi78.01 (16)C9—C13—C12118.3 (5)
O2iv—Dy2—O3W122.91 (16)C9—C13—H13120.8
O11v—Dy2—O3W68.21 (16)C12—C13—H13120.8
O8iii—Dy2—O3W79.91 (17)O7—C14—O8126.2 (5)
O5vi—Dy2—O3W136.70 (16)O7—C14—C12116.8 (5)
O2iv—Dy2—O988.93 (15)O8—C14—C12117.0 (5)
O11v—Dy2—O9150.52 (14)O10—C15—O9122.1 (5)
O8iii—Dy2—O981.60 (15)O10—C15—C16120.2 (5)
O5vi—Dy2—O977.09 (14)O9—C15—C16117.6 (5)
O3W—Dy2—O9135.19 (15)C17—C16—C20117.9 (5)
O2iv—Dy2—O371.25 (15)C17—C16—C15123.0 (5)
O11v—Dy2—O3125.98 (15)C20—C16—C15119.1 (5)
O8iii—Dy2—O3130.93 (16)C16—C17—C18119.0 (5)
O5vi—Dy2—O3139.96 (15)C16—C17—H17120.5
O3W—Dy2—O381.32 (16)C18—C17—H17120.5
O9—Dy2—O380.74 (15)C17—C18—C19118.4 (5)
O2iv—Dy2—O4115.95 (14)C17—C18—C21122.6 (5)
O11v—Dy2—O4142.05 (14)C19—C18—C21118.9 (5)
O8iii—Dy2—O481.94 (14)N3—C19—C18123.2 (6)
O5vi—Dy2—O4137.50 (14)N3—C19—H19118.4
O3W—Dy2—O474.11 (15)C18—C19—H19118.4
O9—Dy2—O463.08 (13)N3—C20—C16123.7 (5)
O3—Dy2—O449.31 (13)N3—C20—H20118.2
C1—O2—Dy2iv151.0 (4)C16—C20—H20118.2
C11—N2—C10116.9 (5)O12—C21—O11126.1 (5)
C3—C2—C6119.2 (5)O12—C21—C18117.6 (5)
C3—C2—C1119.3 (5)O11—C21—C18116.2 (5)
Symmetry codes: (i) x, y+1, z; (ii) x1, y1, z; (iii) x, y, z+1; (iv) x+1, y+1, z; (v) x, y1, z; (vi) x+1, y, z; (vii) x1, y, z; (viii) x, y+1, z; (ix) x+1, y+1, z.
 

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