Poly[[tetra­aqua-μ₂-oxalato-bis­(μ₃-pyridine-3,4-dicarboxyl­ato-κ⁴O,O′:O′′:O′′′)diyttrium(III)] trihydrate]

The title yttrium(III) coordination polymer, {[Y₂(C₇H₃NO₄)₂(C₂O₄)(H₂O)₄]·3H₂O}_n, has a pyridine-3,4-dicarboxyl­ate (PDC) and oxalate (ox) bridged layer-type structure. The central yttrium ion exhibits a distorted dodeca­hedral configuration, coordinated by eight O atoms from three PDC ligands, one ox ligand and two uncoordinated water mol­ecules. The ox ligand lies on a center of inversion.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.005 Å
• H-atom completeness 91%
• Disorder in solvent or counterion
• R factor = 0.035
• wR factor = 0.094
• Data-to-parameter ratio = 13.2

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 ....          ?
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 =          3
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      25.00 Perc.
PLAT369_ALERT_2_C Long   C(sp2)-C(sp2) Bond  C8     -   C8_d   ...       1.53 Ang.
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.26 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:C16 H20 N2 O19 Y2
            Atom count from the _atom_site data:  C16 H18 N2 O19 Y2
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    1
           From the CIF: _chemical_formula_sum  C16 H20 N2 O19 Y2
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C         16.00     16.00    0.00
           H         20.00     18.00    2.00
           N          2.00      2.00    0.00
           O         19.00     19.00    0.00
           Y          2.00      2.00    0.00
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K
PLAT804_ALERT_5_G ARU-Pack Problem in PLATON Analysis ............          1 Times

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

   8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 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
   2 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); 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-Plus.

Poly[[tetraaqua-µ₂-oxalato-bis(µ₃-pyridine-3,4-dicarboxylato- κ⁴O,O':O'':O''')diyttrium(III)] trihydrate]

Crystal data

[Y2(C7H3NO4)2(C2O4)(H2O)4]·3H2O	Z = 1
Mr = 722.16	F(000) = 360
Triclinic, P1	Dx = 1.958 Mg m^−3
Hall symbol: -P1	Mo Kα radiation, λ = 0.71073 Å
a = 5.9785 (3) Å	Cell parameters from 2395 reflections
b = 10.1376 (5) Å	θ = 3.4–26.0°
c = 11.1811 (5) Å	µ = 4.81 mm^−1
α = 104.3400 (5)°	T = 293 K
β = 99.9260 (5)°	Block, yellow
γ = 105.2930 (5)°	0.30 × 0.25 × 0.18 mm
V = 612.47 (5) Å^3

Data collection

Bruker SMART APEXII CCD diffractometer	2395 independent reflections
Radiation source: fine-focus sealed tube	2225 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.097
Detector resolution: 10.0 pixels mm^-1	θmax = 26.0°, θmin = 3.4°
φ and ω scans	h = −7→7
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −12→12
Tmin = 0.246, Tmax = 0.421	l = −13→13
5250 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)] = 0.035	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.094	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0556P)^2] where P = (Fo^2 + 2Fc^2)/3
2395 reflections	(Δ/σ)max = 0.001
181 parameters	Δρmax = 0.96 e Å^−3
0 restraints	Δρmin = −0.85 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	Occ. (<1)
N1	0.8166 (6)	0.3078 (4)	0.4318 (2)	0.0342 (7)
Y1	0.64874 (4)	0.69151 (3)	0.93921 (2)	0.01842 (13)
O1	0.6450 (4)	0.5797 (3)	0.7178 (2)	0.0308 (6)
O1W	0.3979 (4)	0.7273 (3)	1.0725 (2)	0.0306 (5)
H1B	0.4272	0.8029	1.1345	0.037*
H1A	0.2966	0.6641	1.0909	0.037*
O2	0.8478 (4)	0.5210 (2)	0.86906 (19)	0.0223 (5)
O2W	0.3918 (5)	0.7714 (3)	0.8168 (2)	0.0419 (7)
H2A	0.2684	0.7847	0.8389	0.050*
H2B	0.3227	0.7272	0.7384	0.050*
O3W	0.3668 (9)	−0.0370 (5)	0.2501 (4)	0.0976 (14)
H3C	0.2806	0.0025	0.2899	0.117*
H3B	0.4059	0.0359	0.2242	0.117*
O3	1.3356 (4)	0.4774 (3)	0.8838 (2)	0.0341 (6)
O4W	0.600 (3)	−0.0389 (18)	0.4868 (15)	0.157 (6)	0.50
O4	1.0782 (4)	0.2715 (3)	0.8653 (2)	0.0286 (5)
O5	0.9956 (4)	0.8355 (3)	0.9014 (2)	0.0288 (5)
C1	0.7779 (5)	0.5111 (4)	0.7525 (3)	0.0208 (6)
C2	0.8570 (6)	0.4166 (4)	0.6544 (3)	0.0221 (6)
C3	0.7531 (6)	0.3869 (4)	0.5261 (3)	0.0291 (7)
H3A	0.6314	0.4244	0.5043	0.035*
C4	0.9912 (7)	0.2532 (5)	0.4643 (3)	0.0411 (10)
H4A	1.0394	0.1988	0.3999	0.049*
C5	1.1024 (7)	0.2746 (5)	0.5900 (3)	0.0365 (9)
H5A	1.2219	0.2345	0.6091	0.044*
C6	1.0344 (5)	0.3560 (4)	0.6869 (3)	0.0224 (6)
C7	1.1545 (5)	0.3722 (4)	0.8220 (3)	0.0227 (7)
C8	1.0724 (5)	0.9700 (3)	0.9563 (3)	0.0213 (6)
O6	0.7452 (4)	0.9426 (3)	1.0529 (2)	0.0285 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
N1	0.0410 (17)	0.046 (2)	0.0189 (13)	0.0237 (16)	0.0050 (12)	0.0067 (13)
Y1	0.01596 (18)	0.0211 (2)	0.01908 (18)	0.00855 (14)	0.00478 (11)	0.00482 (12)
O1	0.0378 (13)	0.0385 (15)	0.0232 (11)	0.0259 (13)	0.0062 (9)	0.0082 (10)
O1W	0.0295 (12)	0.0268 (14)	0.0384 (12)	0.0093 (11)	0.0204 (10)	0.0070 (10)
O2	0.0236 (11)	0.0268 (13)	0.0197 (10)	0.0130 (10)	0.0061 (8)	0.0071 (9)
O2W	0.0507 (16)	0.065 (2)	0.0198 (11)	0.0448 (16)	0.0047 (10)	0.0058 (12)
O3W	0.113 (4)	0.062 (3)	0.093 (3)	0.011 (3)	0.018 (3)	0.003 (2)
O3	0.0187 (11)	0.0375 (16)	0.0348 (12)	0.0063 (12)	0.0016 (9)	−0.0019 (11)
O4W	0.173 (15)	0.138 (15)	0.197 (14)	0.063 (13)	0.089 (12)	0.074 (12)
O4	0.0283 (12)	0.0352 (15)	0.0250 (11)	0.0123 (12)	0.0055 (9)	0.0123 (10)
O5	0.0294 (12)	0.0239 (13)	0.0373 (12)	0.0101 (11)	0.0185 (10)	0.0080 (10)
C1	0.0188 (14)	0.0224 (17)	0.0214 (14)	0.0082 (13)	0.0055 (11)	0.0054 (12)
C2	0.0208 (15)	0.0270 (18)	0.0213 (14)	0.0110 (15)	0.0067 (12)	0.0078 (13)
C3	0.0324 (17)	0.036 (2)	0.0229 (15)	0.0183 (17)	0.0069 (13)	0.0090 (14)
C4	0.047 (2)	0.059 (3)	0.0238 (16)	0.035 (2)	0.0112 (15)	0.0035 (17)
C5	0.0359 (19)	0.053 (3)	0.0284 (17)	0.030 (2)	0.0081 (14)	0.0094 (17)
C6	0.0189 (14)	0.0258 (18)	0.0203 (14)	0.0070 (14)	0.0036 (11)	0.0044 (13)
C7	0.0159 (14)	0.034 (2)	0.0208 (14)	0.0153 (15)	0.0049 (11)	0.0047 (13)
C8	0.0238 (16)	0.0204 (17)	0.0239 (14)	0.0114 (15)	0.0083 (12)	0.0079 (13)
O6	0.0253 (11)	0.0284 (14)	0.0367 (12)	0.0106 (11)	0.0167 (10)	0.0105 (11)

Geometric parameters (Å, º)

N1—C3	1.334 (4)	O3W—H3C	0.8499
N1—C4	1.342 (4)	O3W—H3B	0.8500
Y1—O2W	2.318 (2)	O3—C7	1.247 (4)
Y1—O3^i	2.322 (3)	O4W—O4W^iii	1.62 (3)
Y1—O1W	2.322 (2)	O4—C7	1.249 (4)
Y1—O5	2.371 (2)	O5—C8	1.267 (4)
Y1—O4^ii	2.372 (2)	C1—C2	1.497 (4)
Y1—O2	2.399 (2)	C2—C3	1.384 (4)
Y1—O6	2.408 (3)	C2—C6	1.399 (4)
Y1—O1	2.447 (2)	C3—H3A	0.9300
Y1—C1	2.777 (3)	C4—C5	1.384 (5)
Y1—O3^ii	2.925 (3)	C4—H4A	0.9300
Y1—C7^ii	3.017 (3)	C5—C6	1.380 (5)
O1—C1	1.259 (4)	C5—H5A	0.9300
O1W—H1B	0.8500	C6—C7	1.504 (4)
O1W—H1A	0.8500	C7—Y1^ii	3.017 (3)
O2—C1	1.268 (3)	C8—O6^iv	1.248 (4)
O2W—H2A	0.8500	C8—C8^iv	1.534 (5)
O2W—H2B	0.8500	O6—C8^iv	1.248 (4)
C3—N1—C4	117.5 (3)	O2—Y1—C7^ii	75.69 (7)
O2W—Y1—O3^i	87.14 (10)	O6—Y1—C7^ii	92.09 (8)
O2W—Y1—O1W	80.49 (8)	O1—Y1—C7^ii	129.45 (8)
O3^i—Y1—O1W	72.80 (9)	C1—Y1—C7^ii	102.71 (8)
O2W—Y1—O5	93.34 (10)	O3^ii—Y1—C7^ii	24.16 (9)
O3^i—Y1—O5	150.67 (8)	C1—O1—Y1	91.26 (17)
O1W—Y1—O5	136.21 (9)	Y1—O1W—H1B	124.7
O2W—Y1—O4^ii	149.60 (9)	Y1—O1W—H1A	127.9
O3^i—Y1—O4^ii	111.21 (9)	H1B—O1W—H1A	103.2
O1W—Y1—O4^ii	82.18 (8)	C1—O2—Y1	93.26 (16)
O5—Y1—O4^ii	82.21 (8)	Y1—O2W—H2A	120.6
O2W—Y1—O2	128.56 (7)	Y1—O2W—H2B	122.9
O3^i—Y1—O2	79.39 (8)	H2A—O2W—H2B	96.6
O1W—Y1—O2	138.60 (8)	H3C—O3W—H3B	88.0
O5—Y1—O2	77.48 (8)	C7—O3—Y1^v	161.8 (2)
O4^ii—Y1—O2	80.00 (8)	C7—O3—Y1^ii	82.1 (2)
O2W—Y1—O6	75.21 (9)	Y1^v—O3—Y1^ii	115.96 (9)
O3^i—Y1—O6	139.64 (8)	C7—O4—Y1^ii	108.9 (2)
O1W—Y1—O6	68.69 (8)	C8—O5—Y1	119.88 (18)
O5—Y1—O6	67.83 (7)	O1—C1—O2	121.4 (3)
O4^ii—Y1—O6	75.28 (8)	O1—C1—C2	119.4 (2)
O2—Y1—O6	139.48 (8)	O2—C1—C2	119.2 (2)
O2W—Y1—O1	74.64 (7)	O1—C1—Y1	61.78 (15)
O3^i—Y1—O1	78.25 (9)	O2—C1—Y1	59.61 (14)
O1W—Y1—O1	142.47 (9)	C2—C1—Y1	177.9 (2)
O5—Y1—O1	73.65 (9)	C3—C2—C6	117.8 (3)
O4^ii—Y1—O1	131.34 (7)	C3—C2—C1	119.7 (3)
O2—Y1—O1	54.09 (7)	C6—C2—C1	122.6 (3)
O6—Y1—O1	128.75 (8)	N1—C3—C2	124.1 (3)
O2W—Y1—C1	101.55 (8)	N1—C3—H3A	117.9
O3^i—Y1—C1	77.79 (9)	C2—C3—H3A	117.9
O1W—Y1—C1	150.40 (10)	N1—C4—C5	122.6 (3)
O5—Y1—C1	73.38 (9)	N1—C4—H4A	118.7
O4^ii—Y1—C1	105.83 (8)	C5—C4—H4A	118.7
O2—Y1—C1	27.13 (8)	C6—C5—C4	119.4 (3)
O6—Y1—C1	140.71 (8)	C6—C5—H5A	120.3
O1—Y1—C1	26.96 (8)	C4—C5—H5A	120.3
O2W—Y1—O3^ii	142.60 (9)	C5—C6—C2	118.6 (3)
O3^i—Y1—O3^ii	64.04 (9)	C5—C6—C7	117.5 (3)
O1W—Y1—O3^ii	68.91 (7)	C2—C6—C7	123.9 (3)
O5—Y1—O3^ii	123.58 (7)	O3—C7—O4	121.7 (3)
O4^ii—Y1—O3^ii	47.17 (8)	O3—C7—C6	120.5 (3)
O2—Y1—O3^ii	71.55 (6)	O4—C7—C6	117.6 (3)
O6—Y1—O3^ii	110.93 (7)	O3—C7—Y1^ii	73.79 (18)
O1—Y1—O3^ii	118.26 (8)	O4—C7—Y1^ii	48.06 (15)
C1—Y1—O3^ii	95.31 (8)	C6—C7—Y1^ii	162.9 (2)
O2W—Y1—C7^ii	153.70 (8)	O6^iv—C8—O5	126.4 (3)
O3^i—Y1—C7^ii	88.18 (9)	O6^iv—C8—C8^iv	117.3 (4)
O1W—Y1—C7^ii	73.40 (8)	O5—C8—C8^iv	116.3 (3)
O5—Y1—C7^ii	103.19 (8)	C8^iv—O6—Y1	118.70 (18)
O4^ii—Y1—C7^ii	23.06 (9)

Symmetry codes: (i) x−1, y, z; (ii) −x+2, −y+1, −z+2; (iii) −x+1, −y, −z+1; (iv) −x+2, −y+2, −z+2; (v) x+1, y, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1A···O2^vi	0.85	2.04	2.849 (4)	159 (4)
O1W—H1B···O3W^vii	0.85	1.97	2.775 (5)	158 (3)
O2W—H2A···O5^i	0.85	2.02	2.865 (4)	175 (2)
O2W—H2B···N1^viii	0.85	1.84	2.662 (3)	161 (6)

Symmetry codes: (i) x−1, y, z; (vi) −x+1, −y+1, −z+2; (vii) x, y+1, z+1; (viii) −x+1, −y+1, −z+1.