catena-Poly[[[diaqua­(6-carboxy­pyridine-2-carboxyl­ato-κ³O,N,O′)erbium(III)]-μ-pyridine-2,6-dicarboxyl­ato-κ⁴O,N,O′:O] tetra­hydrate]

In the title structure, {[Er(C₇H₃NO₄)(C₇H₄NO₄)(H₂O)₂]·4H₂O}_n, the Er^III atom is nine-coordin­ated by a tridendate pyridine-2,6-dicarboxyl­ate (pdc) ligand, a tridentate 6-carboxy­pyridine-2-carboxyl­ate ligand (Hpdc), two water mol­ecules and a bridging carboxyl­ate O atom from a symmetry-related ligand, forming a one-dimensional chain structure propagating along the c axis. In the crystal structure, inter­molecular O—H...O hydrogen bonds link these chains into a three-dimensional network.

Key indicators

• Single-crystal X-ray study
• T = 292 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.031
• wR factor = 0.086
• Data-to-parameter ratio = 15.3

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT220_ALERT_2_B Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.56 Ratio
PLAT355_ALERT_3_B Long    O-H Bond (0.82A)   O13    -   H13A   ...       1.09 Ang.

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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 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

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Computing details

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); 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, 2000); software used to prepare material for publication: SHELXTL.

catena-poly[[[diaqua(6-carboxypyridine-2-carboxylato-κ³O,N,O')erbium(III)]- µ-pyridine-2,6-dicarboxylato-κ⁴O,N,O':O] tetrahydrate]

Crystal data

[Er(C7H3NO4)(C7H4NO4)(H2O)2]·4H2O	F(000) = 1188
Mr = 606.57	Dx = 2.051 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 5265 reflections
a = 13.9915 (15) Å	θ = 2.4–28.3°
b = 11.2079 (12) Å	µ = 4.35 mm^−1
c = 12.8282 (14) Å	T = 292 K
β = 102.439 (2)°	Block, colourless
V = 1964.4 (4) Å^3	0.20 × 0.10 × 0.10 mm
Z = 4

Data collection

Bruker SMART CCD diffractometer	4276 independent reflections
Radiation source: fine-focus sealed tube	3976 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.047
φ and ω scans	θmax = 27.0°, θmin = 1.5°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −17→17
Tmin = 0.462, Tmax = 0.650	k = −12→14
16162 measured reflections	l = −16→16

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)] = 0.031	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.086	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0536P)^2 + 3.616P] where P = (Fo^2 + 2Fc^2)/3
4276 reflections	(Δ/σ)max = 0.001
280 parameters	Δρmax = 1.04 e Å^−3
0 restraints	Δρmin = −0.81 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
Er1	0.729855 (12)	0.795913 (15)	0.351028 (13)	0.01823 (8)
O1	0.5161 (3)	1.1015 (3)	0.3732 (3)	0.0380 (8)
H1O	0.5671	1.1465	0.3986	0.046*
O2	0.6468 (2)	0.9921 (3)	0.3635 (2)	0.0253 (6)
O3	0.6582 (2)	0.6005 (2)	0.3673 (2)	0.0219 (6)
O4	0.5340 (2)	0.4797 (3)	0.3754 (3)	0.0342 (7)
O5	0.7796 (2)	0.8291 (3)	0.7166 (2)	0.0213 (6)
O6	0.7254 (2)	0.7784 (2)	0.5448 (2)	0.0192 (6)
O7	0.8420 (2)	0.9264 (2)	0.2797 (2)	0.0233 (6)
O8	0.9178 (3)	1.1023 (3)	0.2827 (2)	0.0334 (7)
O9	0.8726 (2)	0.6884 (3)	0.4350 (2)	0.0260 (7)
H9A	0.8958	0.6913	0.4997	0.031*
H9B	0.8972	0.6348	0.4065	0.031*
O10	0.6327 (2)	0.8453 (3)	0.1758 (2)	0.0308 (7)
H10A	0.5912	0.8966	0.1690	0.037*
H10B	0.6542	0.8327	0.1228	0.037*
N3	0.5506 (2)	0.7909 (3)	0.3668 (3)	0.0185 (7)
N4	0.8306 (2)	0.9455 (3)	0.4806 (2)	0.0137 (6)
C1	0.4993 (3)	0.8924 (4)	0.3654 (3)	0.0239 (8)
C2	0.4000 (4)	0.8926 (5)	0.3628 (4)	0.0408 (12)
H2	0.3656	0.9639	0.3607	0.049*
C3	0.3537 (4)	0.7848 (5)	0.3635 (6)	0.0520 (16)
H3	0.2868	0.7825	0.3611	0.062*
C4	0.4062 (4)	0.6792 (5)	0.3678 (5)	0.0402 (12)
H4	0.3762	0.6055	0.3699	0.048*
C5	0.5056 (3)	0.6879 (4)	0.3686 (3)	0.0223 (8)
C6	0.5607 (3)	1.0018 (4)	0.3672 (3)	0.0243 (8)
C7	0.5706 (3)	0.5804 (4)	0.3715 (3)	0.0210 (8)
C8	0.8254 (3)	0.9486 (3)	0.5838 (3)	0.0149 (7)
C9	0.8613 (3)	1.0436 (4)	0.6500 (3)	0.0206 (8)
H9	0.8586	1.0427	0.7218	0.025*
C10	0.9009 (3)	1.1388 (4)	0.6072 (3)	0.0248 (8)
H10	0.9238	1.2046	0.6494	0.030*
C11	0.9065 (3)	1.1364 (3)	0.5002 (3)	0.0220 (8)
H11	0.9329	1.2004	0.4698	0.026*
C12	0.8720 (3)	1.0369 (3)	0.4404 (3)	0.0163 (7)
C13	0.7732 (3)	0.8438 (3)	0.6192 (3)	0.0146 (7)
C14	0.8780 (3)	1.0222 (4)	0.3242 (3)	0.0205 (8)
O11	0.9587 (2)	0.6931 (3)	0.6480 (2)	0.0284 (7)
H11A	0.9840	0.7592	0.6572	0.034*
H11B	0.9409	0.6684	0.7004	0.034*
O12	0.6283 (3)	0.2745 (3)	0.3879 (4)	0.0610 (13)
H12A	0.5977	0.3367	0.3759	0.073*
H12B	0.6741	0.2960	0.3473	0.073*
O13	0.8019 (3)	0.4040 (4)	0.4112 (4)	0.0710 (14)
H13A	0.7932	0.4205	0.4925	0.085*
H13B	0.7815	0.4690	0.3874	0.085*
O14	0.9713 (2)	0.4420 (3)	0.5975 (3)	0.0352 (7)
H14A	0.9889	0.5117	0.6032	0.042*
H14B	0.9516	0.4184	0.6492	0.042*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Er1	0.02110 (12)	0.01789 (12)	0.01640 (11)	−0.00013 (6)	0.00559 (8)	−0.00080 (6)
O1	0.0394 (19)	0.0247 (17)	0.049 (2)	0.0116 (14)	0.0069 (16)	−0.0065 (15)
O2	0.0276 (15)	0.0161 (14)	0.0321 (15)	0.0039 (11)	0.0060 (12)	−0.0025 (12)
O3	0.0218 (14)	0.0151 (13)	0.0298 (15)	0.0001 (10)	0.0081 (11)	−0.0010 (11)
O4	0.0295 (16)	0.0204 (15)	0.053 (2)	−0.0076 (13)	0.0088 (15)	0.0001 (14)
O5	0.0306 (15)	0.0211 (13)	0.0130 (12)	−0.0056 (12)	0.0067 (11)	0.0021 (11)
O6	0.0259 (15)	0.0190 (13)	0.0133 (12)	−0.0087 (11)	0.0058 (11)	−0.0015 (10)
O7	0.0345 (16)	0.0229 (14)	0.0157 (12)	−0.0100 (12)	0.0125 (11)	−0.0051 (11)
O8	0.054 (2)	0.0271 (16)	0.0252 (15)	−0.0170 (14)	0.0214 (14)	−0.0004 (13)
O9	0.0293 (16)	0.0303 (16)	0.0160 (13)	0.0109 (12)	−0.0004 (12)	−0.0052 (11)
O10	0.0350 (17)	0.0411 (19)	0.0160 (13)	0.0203 (14)	0.0052 (12)	−0.0018 (13)
N3	0.0183 (16)	0.0213 (18)	0.0167 (15)	0.0017 (12)	0.0053 (13)	0.0001 (12)
N4	0.0176 (14)	0.0122 (14)	0.0122 (13)	−0.0018 (11)	0.0054 (11)	−0.0002 (11)
C1	0.024 (2)	0.026 (2)	0.0225 (19)	0.0091 (16)	0.0069 (15)	0.0001 (16)
C2	0.029 (2)	0.039 (3)	0.058 (3)	0.015 (2)	0.019 (2)	0.002 (2)
C3	0.026 (3)	0.049 (3)	0.086 (5)	0.006 (2)	0.024 (3)	0.008 (3)
C4	0.023 (2)	0.038 (3)	0.064 (4)	−0.0029 (19)	0.018 (2)	0.006 (3)
C5	0.019 (2)	0.024 (2)	0.025 (2)	0.0017 (15)	0.0078 (16)	−0.0003 (16)
C6	0.034 (2)	0.019 (2)	0.0196 (18)	0.0085 (16)	0.0045 (16)	−0.0027 (15)
C7	0.0211 (19)	0.022 (2)	0.0201 (18)	−0.0025 (15)	0.0052 (15)	−0.0020 (15)
C8	0.0169 (17)	0.0140 (17)	0.0140 (16)	−0.0006 (13)	0.0041 (13)	0.0000 (13)
C9	0.0259 (19)	0.0214 (19)	0.0141 (16)	−0.0021 (15)	0.0034 (14)	−0.0008 (14)
C10	0.032 (2)	0.021 (2)	0.0212 (19)	−0.0097 (16)	0.0059 (16)	−0.0061 (16)
C11	0.030 (2)	0.0172 (19)	0.0202 (18)	−0.0060 (15)	0.0082 (16)	−0.0001 (15)
C12	0.0205 (17)	0.0150 (17)	0.0142 (16)	−0.0017 (13)	0.0056 (13)	0.0011 (13)
C13	0.0181 (17)	0.0135 (17)	0.0135 (15)	0.0017 (13)	0.0063 (13)	0.0011 (14)
C14	0.027 (2)	0.0194 (19)	0.0182 (17)	−0.0029 (15)	0.0106 (15)	0.0005 (15)
O11	0.0321 (17)	0.0338 (18)	0.0201 (14)	−0.0035 (12)	0.0075 (13)	0.0022 (12)
O12	0.063 (3)	0.0256 (19)	0.098 (4)	0.0037 (18)	0.025 (3)	−0.001 (2)
O13	0.062 (3)	0.037 (2)	0.105 (4)	0.012 (2)	−0.003 (3)	−0.003 (2)
O14	0.048 (2)	0.0314 (17)	0.0325 (17)	0.0086 (15)	0.0223 (15)	0.0033 (14)

Geometric parameters (Å, º)

Er1—O9	2.382 (3)	C1—C2	1.382 (6)
Er1—O10	2.427 (3)	C1—C6	1.495 (6)
Er1—O3	2.436 (3)	C2—C3	1.372 (8)
Er1—O5^i	2.437 (3)	C2—H2	0.9300
Er1—O7	2.461 (3)	C3—C4	1.388 (7)
Er1—O6	2.507 (3)	C3—H3	0.9300
Er1—O2	2.508 (3)	C4—C5	1.391 (6)
Er1—N3	2.559 (3)	C4—H4	0.9300
Er1—N4	2.560 (3)	C5—C7	1.506 (5)
O1—C6	1.291 (5)	C8—C9	1.386 (5)
O1—H1O	0.8769	C8—C13	1.504 (5)
O2—C6	1.221 (5)	C9—C10	1.370 (6)
O3—C7	1.259 (5)	C9—H9	0.9300
O4—C7	1.244 (5)	C10—C11	1.392 (5)
O5—C13	1.245 (4)	C10—H10	0.9300
O5—Er1^ii	2.437 (3)	C11—C12	1.381 (5)
O6—C13	1.273 (5)	C11—H11	0.9300
O7—C14	1.267 (5)	C12—C14	1.519 (5)
O8—C14	1.237 (5)	O11—H11A	0.8187
O9—H9A	0.8243	O11—H11B	0.8138
O9—H9B	0.8161	O12—H12A	0.8152
O10—H10A	0.8084	O12—H12B	0.9406
O10—H10B	0.8129	O13—H13A	1.0906
N3—C5	1.317 (5)	O13—H13B	0.8171
N3—C1	1.344 (5)	O14—H14A	0.8177
N4—C12	1.335 (4)	O14—H14B	0.8153
N4—C8	1.342 (4)
O9—Er1—O10	141.43 (10)	C1—N3—Er1	120.7 (3)
O9—Er1—O3	80.01 (10)	C12—N4—C8	118.8 (3)
O10—Er1—O3	97.21 (11)	C12—N4—Er1	118.4 (2)
O9—Er1—O5^i	71.91 (10)	C8—N4—Er1	121.2 (2)
O10—Er1—O5^i	70.37 (10)	N3—C1—C2	122.3 (4)
O3—Er1—O5^i	74.28 (9)	N3—C1—C6	113.0 (3)
O9—Er1—O7	85.96 (11)	C2—C1—C6	124.8 (4)
O10—Er1—O7	78.16 (11)	C3—C2—C1	118.1 (4)
O3—Er1—O7	150.83 (9)	C3—C2—H2	120.9
O5^i—Er1—O7	77.10 (9)	C1—C2—H2	120.9
O9—Er1—O6	73.12 (10)	C2—C3—C4	120.3 (5)
O10—Er1—O6	143.84 (10)	C2—C3—H3	119.8
O3—Er1—O6	75.29 (9)	C4—C3—H3	119.8
O5^i—Er1—O6	136.74 (9)	C3—C4—C5	117.4 (5)
O7—Er1—O6	124.69 (9)	C3—C4—H4	121.3
O9—Er1—O2	140.32 (10)	C5—C4—H4	121.3
O10—Er1—O2	71.60 (10)	N3—C5—C4	122.9 (4)
O3—Er1—O2	125.30 (10)	N3—C5—C7	114.4 (3)
O5^i—Er1—O2	139.12 (9)	C4—C5—C7	122.8 (4)
O7—Er1—O2	81.01 (9)	O2—C6—O1	125.0 (4)
O6—Er1—O2	83.96 (9)	O2—C6—C1	119.7 (4)
O9—Er1—N3	133.87 (11)	O1—C6—C1	115.3 (4)
O10—Er1—N3	73.48 (10)	O4—C7—O3	125.3 (4)
O3—Er1—N3	62.95 (9)	O4—C7—C5	118.3 (4)
O5^i—Er1—N3	118.52 (10)	O3—C7—C5	116.3 (3)
O7—Er1—N3	139.15 (10)	N4—C8—C9	122.3 (3)
O6—Er1—N3	71.67 (10)	N4—C8—C13	114.2 (3)
O2—Er1—N3	62.55 (10)	C9—C8—C13	123.5 (3)
O9—Er1—N4	75.35 (10)	C10—C9—C8	118.5 (3)
O10—Er1—N4	124.92 (11)	C10—C9—H9	120.7
O3—Er1—N4	135.43 (9)	C8—C9—H9	120.7
O5^i—Er1—N4	129.41 (10)	C9—C10—C11	119.6 (4)
O7—Er1—N4	63.00 (9)	C9—C10—H10	120.2
O6—Er1—N4	62.32 (9)	C11—C10—H10	120.2
O2—Er1—N4	65.32 (10)	C12—C11—C10	118.5 (3)
N3—Er1—N4	112.01 (10)	C12—C11—H11	120.8
C6—O1—H1O	98.9	C10—C11—H11	120.8
C6—O2—Er1	123.7 (3)	N4—C12—C11	122.2 (3)
C7—O3—Er1	126.0 (3)	N4—C12—C14	114.6 (3)
C13—O5—Er1^ii	144.7 (3)	C11—C12—C14	123.2 (3)
C13—O6—Er1	125.2 (2)	O5—C13—O6	126.1 (3)
C14—O7—Er1	124.0 (2)	O5—C13—C8	118.1 (3)
Er1—O9—H9A	123.1	O6—C13—C8	115.8 (3)
Er1—O9—H9B	124.2	O8—C14—O7	126.3 (3)
H9A—O9—H9B	111.6	O8—C14—C12	117.9 (3)
Er1—O10—H10A	120.5	O7—C14—C12	115.7 (3)
Er1—O10—H10B	120.1	H11A—O11—H11B	112.9
H10A—O10—H10B	114.8	H12A—O12—H12B	94.0
C5—N3—C1	119.0 (4)	H13A—O13—H13B	96.0
C5—N3—Er1	120.1 (2)	H14A—O14—H14B	112.7

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
O1—H1O···O12^iii	0.88	1.69	2.476 (6)	147
O9—H9A···O11	0.82	1.92	2.738 (4)	176
O9—H9B···O14^iv	0.82	2.04	2.734 (4)	142
O10—H10A···O4^v	0.81	1.96	2.735 (4)	161
O10—H10B···O6^i	0.81	1.99	2.714 (4)	148
O11—H11A···O8^vi	0.82	2.11	2.894 (4)	161
O11—H11B···O7^ii	0.81	2.17	2.917 (4)	154
O12—H12A···O4	0.82	1.83	2.640 (5)	170
O12—H12B···O13	0.94	2.17	2.790 (7)	123
O13—H13A···O14	1.09	2.58	3.012 (6)	103
O13—H13B···O3	0.82	2.24	2.953 (5)	146
O14—H14A···O11	0.82	2.18	2.902 (4)	148
O14—H14B···O8^ii	0.82	1.89	2.686 (4)	167

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