Poly[μ₄-acetyl­acetonato-di-μ₃-acetyl­acetonato-pyridinetrisodium(I)]

In the title compound, [Na₃(C₅H₇O₂)₃(C₅H₅N)]_n, the two O atoms of one acetyl­acetonate (acac) ligand bridge four Na atoms in a μ₃ fashion, whereas the two other independent acac ligands bridge three Na atoms each, in a μ₂-fashion. All three Na atoms are in distorted square-pyramidal edge-sharing coordin­ation polyhedra. The resulting assemblage is a polymeric chain directed along the c axis. This is the first example of Na—μ₃-O(acac) bonds to be reported.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.050
• wR factor = 0.125
• Data-to-parameter ratio = 15.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.28 Ratio

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   1 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
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: COLLECT (Nonius, 1998); cell refinement: HKL-2000 (Otwinowski & Minor, 1997); data reduction: HKL-2000; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1999); software used to prepare material for publication: SHELXTL and PLATON (Spek, 2003).

poly[tri-µ₃-acetylacetonato-pytidinetrisodium(I)]

Crystal data

[Na3(C5H7O2)3(C5H5N)]	F(000) = 936
Mr = 445.39	Dx = 1.273 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 16242 reflections
a = 10.8858 (13) Å	θ = 2.1–25.7°
b = 18.969 (2) Å	µ = 0.14 mm^−1
c = 12.1338 (12) Å	T = 100 K
β = 111.941 (7)°	Irregular, colourless
V = 2324.1 (5) Å^3	0.14 × 0.12 × 0.09 mm
Z = 4

Data collection

Nonius KappaCCD area-detector diffractometer	2999 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.065
Graphite monochromator	θmax = 25.7°, θmin = 2.1°
φ scan with 2° steps	h = 0→13
16242 measured reflections	k = 0→23
4353 independent reflections	l = −14→13

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)] = 0.050	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.126	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0521P)^2 + 0.6412P] where P = (Fo^2 + 2Fc^2)/3
4353 reflections	(Δ/σ)max < 0.001
277 parameters	Δρmax = 0.17 e Å^−3
0 restraints	Δρmin = −0.24 e Å^−3

Special details

Experimental. crystal-to-detector distance 30 mm

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. Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH₃) times that of the parent atom. 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
Na1	0.67782 (10)	0.07025 (5)	0.70263 (8)	0.0409 (3)
Na2	0.51509 (10)	0.06945 (5)	0.41192 (9)	0.0428 (3)
Na3	0.52947 (10)	−0.00977 (5)	0.87299 (8)	0.0391 (3)
O1	0.66005 (18)	−0.00587 (9)	0.54916 (15)	0.0418 (4)
O2	0.67105 (18)	−0.04351 (9)	0.77762 (15)	0.0414 (4)
O3	0.55536 (19)	0.10101 (9)	0.80662 (16)	0.0456 (4)
O4	0.52702 (18)	0.14394 (9)	0.56849 (15)	0.0436 (4)
O5	0.64935 (17)	0.01639 (9)	1.07117 (14)	0.0406 (4)
O6	0.61308 (18)	0.08015 (9)	1.27572 (15)	0.0443 (4)
N1	0.8887 (2)	0.12571 (11)	0.73372 (18)	0.0437 (5)
C1	0.7965 (3)	−0.07008 (15)	0.4716 (3)	0.0539 (7)
H1A	0.7227	−0.0769	0.3981	0.081*
H1B	0.8496	−0.1120	0.4908	0.081*
H1C	0.8491	−0.0312	0.4637	0.081*
C2	0.7463 (3)	−0.05450 (13)	0.5693 (2)	0.0418 (6)
C3	0.7951 (3)	−0.09427 (13)	0.6744 (2)	0.0426 (6)
H3	0.8599	−0.1276	0.6804	0.051*
C4	0.7545 (3)	−0.08808 (12)	0.7715 (2)	0.0394 (6)
C5	0.8112 (3)	−0.13842 (14)	0.8743 (2)	0.0473 (7)
H5A	0.8699	−0.1134	0.9424	0.071*
H5B	0.8592	−0.1751	0.8532	0.071*
H5C	0.7405	−0.1589	0.8927	0.071*
C6	0.4969 (3)	0.18500 (16)	0.9221 (3)	0.0609 (8)
H6A	0.4301	0.1572	0.9353	0.091*
H6B	0.4723	0.2339	0.9165	0.091*
H6C	0.5800	0.1786	0.9870	0.091*
C7	0.5102 (3)	0.16187 (14)	0.8070 (2)	0.0439 (6)
C8	0.4701 (3)	0.20861 (13)	0.7104 (2)	0.0449 (6)
H8	0.4392	0.2525	0.7225	0.054*
C9	0.4720 (3)	0.19551 (13)	0.5969 (2)	0.0434 (6)
C10	0.4007 (3)	0.24749 (15)	0.4991 (3)	0.0556 (8)
H10A	0.4605	0.2643	0.4636	0.083*
H10B	0.3697	0.2865	0.5320	0.083*
H10C	0.3268	0.2246	0.4398	0.083*
C11	0.8441 (3)	0.05105 (14)	1.0420 (2)	0.0452 (6)
H11A	0.8466	0.0047	1.0110	0.068*
H11B	0.9320	0.0651	1.0920	0.068*
H11C	0.8092	0.0838	0.9775	0.068*
C12	0.7562 (3)	0.05029 (13)	1.1139 (2)	0.0391 (6)
C13	0.8006 (3)	0.08803 (13)	1.2213 (2)	0.0413 (6)
H13	0.8847	0.1078	1.2449	0.050*
C14	0.7312 (3)	0.09903 (13)	1.2967 (2)	0.0419 (6)
C15	0.8015 (3)	0.13651 (15)	1.4135 (2)	0.0508 (7)
H15A	0.7511	0.1771	1.4183	0.076*
H15B	0.8878	0.1511	1.4183	0.076*
H15C	0.8101	0.1051	1.4780	0.076*
C16	1.0026 (3)	0.09108 (15)	0.7556 (2)	0.0495 (7)
H16	1.0035	0.0426	0.7676	0.059*
C17	1.1183 (3)	0.12289 (17)	0.7612 (3)	0.0566 (8)
H17	1.1954	0.0967	0.7786	0.068*
C18	1.1175 (3)	0.19442 (17)	0.7407 (3)	0.0569 (8)
H18	1.1939	0.2173	0.7427	0.068*
C19	1.0020 (3)	0.23123 (15)	0.7173 (3)	0.0534 (7)
H19	0.9987	0.2795	0.7034	0.064*
C20	0.8906 (3)	0.19509 (14)	0.7148 (2)	0.0483 (7)
H20	0.8127	0.2204	0.6990	0.058*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Na1	0.0444 (6)	0.0387 (5)	0.0406 (5)	0.0005 (4)	0.0170 (5)	−0.0019 (4)
Na2	0.0438 (6)	0.0470 (6)	0.0386 (5)	−0.0030 (5)	0.0165 (5)	−0.0015 (4)
Na3	0.0395 (6)	0.0419 (5)	0.0366 (5)	−0.0020 (4)	0.0150 (4)	−0.0013 (4)
O1	0.0442 (11)	0.0406 (10)	0.0421 (10)	0.0007 (8)	0.0180 (9)	−0.0036 (8)
O2	0.0437 (11)	0.0395 (9)	0.0420 (10)	0.0032 (8)	0.0172 (8)	−0.0009 (8)
O3	0.0544 (12)	0.0388 (10)	0.0483 (10)	0.0068 (9)	0.0246 (9)	0.0028 (8)
O4	0.0484 (11)	0.0391 (10)	0.0422 (10)	0.0005 (8)	0.0158 (9)	−0.0008 (8)
O5	0.0377 (10)	0.0465 (10)	0.0374 (9)	−0.0060 (8)	0.0136 (8)	−0.0020 (8)
O6	0.0458 (11)	0.0496 (11)	0.0389 (10)	−0.0093 (9)	0.0175 (9)	−0.0057 (8)
N1	0.0449 (14)	0.0446 (13)	0.0401 (12)	0.0012 (10)	0.0140 (10)	−0.0019 (10)
C1	0.0582 (19)	0.0580 (17)	0.0548 (17)	0.0047 (15)	0.0318 (16)	−0.0058 (14)
C2	0.0396 (15)	0.0403 (14)	0.0470 (15)	−0.0065 (12)	0.0180 (13)	−0.0084 (12)
C3	0.0375 (15)	0.0408 (14)	0.0484 (15)	0.0008 (12)	0.0148 (12)	−0.0033 (12)
C4	0.0343 (14)	0.0342 (13)	0.0468 (15)	−0.0021 (11)	0.0118 (12)	−0.0033 (11)
C5	0.0463 (17)	0.0399 (14)	0.0528 (16)	0.0009 (12)	0.0150 (13)	0.0015 (12)
C6	0.072 (2)	0.0615 (19)	0.0527 (18)	0.0195 (17)	0.0274 (17)	−0.0031 (15)
C7	0.0451 (16)	0.0406 (14)	0.0476 (15)	0.0034 (12)	0.0191 (13)	−0.0022 (12)
C8	0.0484 (17)	0.0342 (13)	0.0515 (16)	0.0015 (12)	0.0178 (13)	−0.0030 (12)
C9	0.0427 (16)	0.0343 (13)	0.0505 (16)	−0.0034 (12)	0.0141 (13)	0.0000 (12)
C10	0.060 (2)	0.0449 (16)	0.0492 (17)	0.0009 (14)	0.0059 (15)	0.0017 (13)
C11	0.0392 (15)	0.0504 (15)	0.0469 (15)	−0.0060 (12)	0.0171 (13)	−0.0029 (12)
C12	0.0378 (15)	0.0391 (13)	0.0390 (14)	−0.0021 (12)	0.0125 (12)	0.0041 (11)
C13	0.0388 (15)	0.0407 (14)	0.0426 (14)	−0.0082 (11)	0.0131 (12)	−0.0036 (11)
C14	0.0458 (17)	0.0390 (14)	0.0381 (14)	−0.0072 (12)	0.0127 (12)	−0.0003 (11)
C15	0.0554 (19)	0.0509 (16)	0.0435 (15)	−0.0111 (14)	0.0154 (14)	−0.0076 (13)
C16	0.0509 (18)	0.0512 (16)	0.0457 (16)	0.0039 (14)	0.0173 (14)	−0.0014 (13)
C17	0.0514 (19)	0.067 (2)	0.0526 (17)	0.0095 (15)	0.0214 (15)	−0.0042 (15)
C18	0.0512 (19)	0.071 (2)	0.0512 (17)	−0.0104 (16)	0.0218 (15)	−0.0063 (15)
C19	0.059 (2)	0.0469 (16)	0.0521 (17)	−0.0076 (14)	0.0178 (15)	−0.0019 (13)
C20	0.0511 (18)	0.0417 (15)	0.0499 (16)	−0.0011 (13)	0.0162 (14)	−0.0050 (12)

Geometric parameters (Å, º)

Na1—O1	2.307 (2)	C2—C3	1.403 (4)
Na1—O2	2.354 (2)	C3—C4	1.410 (3)
Na1—O3	2.229 (2)	C3—H3	0.9300
Na1—O4	2.302 (2)	C4—C5	1.508 (4)
Na1—N1	2.423 (2)	C5—H5A	0.9600
Na1—Na2	3.3032 (14)	C5—H5B	0.9600
Na1—Na2^i	3.3442 (14)	C5—H5C	0.9600
Na1—Na3	3.4175 (13)	C6—C7	1.522 (4)
Na2—O1	2.311 (2)	C6—H6A	0.9600
Na2—O1^i	2.447 (2)	C6—H6B	0.9600
Na2—O2^i	2.481 (2)	C6—H6C	0.9600
Na2—O4	2.332 (2)	C7—C8	1.403 (4)
Na2—O6^ii	2.286 (2)	C8—C9	1.407 (4)
Na2—Na2^i	3.4850 (19)	C8—H8	0.9300
Na2—Na3^i	3.4949 (13)	C9—C10	1.514 (4)
Na3—O2	2.336 (2)	C10—H10A	0.9600
Na3—O3	2.305 (2)	C10—H10B	0.9600
Na3—O5	2.321 (2)	C10—H10C	0.9600
Na3—O5^iii	2.291 (2)	C11—C12	1.516 (3)
Na3—O6^iii	2.314 (2)	C11—H11A	0.9600
Na3—Na3^iii	3.3953 (18)	C11—H11B	0.9600
O1—C2	1.273 (3)	C11—H11C	0.9600
O1—Na2^i	2.447 (2)	C12—C13	1.405 (3)
O2—C4	1.264 (3)	C13—C14	1.403 (3)
O2—Na2^i	2.481 (2)	C13—H13	0.9300
O3—C7	1.255 (3)	C14—C15	1.513 (4)
O4—C9	1.260 (3)	C15—H15A	0.9600
O5—C12	1.259 (3)	C15—H15B	0.9600
O5—Na3^iii	2.2913 (19)	C15—H15C	0.9600
O6—C14	1.266 (3)	C16—C17	1.375 (4)
O6—Na2^iv	2.2864 (18)	C16—H16	0.9300
O6—Na3^iii	2.314 (2)	C17—C18	1.379 (4)
N1—C20	1.338 (3)	C17—H17	0.9300
N1—C16	1.339 (3)	C18—C19	1.372 (4)
C1—C2	1.509 (3)	C18—H18	0.9300
C1—H1A	0.9600	C19—C20	1.384 (4)
C1—H1B	0.9600	C19—H19	0.9300
C1—H1C	0.9600	C20—H20	0.9300
O3—Na1—O4	79.74 (7)	C4—C3—H3	117.1
O3—Na1—O1	137.18 (8)	O2—C4—C3	124.2 (2)
O4—Na1—O1	89.24 (7)	O2—C4—C5	117.1 (2)
O3—Na1—O2	84.80 (7)	C3—C4—C5	118.7 (2)
O4—Na1—O2	135.47 (8)	C4—C5—H5A	109.5
O1—Na1—O2	74.51 (6)	C4—C5—H5B	109.5
O3—Na1—N1	122.04 (8)	H5A—C5—H5B	109.5
O4—Na1—N1	103.31 (8)	C4—C5—H5C	109.5
O1—Na1—N1	100.73 (7)	H5A—C5—H5C	109.5
O2—Na1—N1	120.16 (8)	H5B—C5—H5C	109.5
O6^ii—Na2—O1	101.44 (7)	C7—C6—H6A	109.5
O6^ii—Na2—O4	129.50 (7)	C7—C6—H6B	109.5
O1—Na2—O4	88.42 (7)	H6A—C6—H6B	109.5
O6^ii—Na2—O1^i	142.28 (7)	C7—C6—H6C	109.5
O1—Na2—O1^i	85.85 (7)	H6A—C6—H6C	109.5
O4—Na2—O1^i	87.23 (7)	H6B—C6—H6C	109.5
O6^ii—Na2—O2^i	77.74 (7)	O3—C7—C8	125.3 (2)
O1—Na2—O2^i	130.29 (7)	O3—C7—C6	116.1 (2)
O4—Na2—O2^i	130.77 (7)	C8—C7—C6	118.6 (2)
O1^i—Na2—O2^i	69.86 (6)	C7—C8—C9	126.3 (2)
O5^iii—Na3—O3	112.43 (7)	C7—C8—H8	116.8
O5^iii—Na3—O6^iii	78.62 (7)	C9—C8—H8	116.8
O3—Na3—O6^iii	112.80 (7)	O4—C9—C8	125.9 (2)
O5^iii—Na3—O5	85.19 (7)	O4—C9—C10	116.6 (2)
O3—Na3—O5	94.14 (7)	C8—C9—C10	117.4 (2)
O6^iii—Na3—O5	152.25 (7)	C9—C10—H10A	109.5
O5^iii—Na3—O2	157.25 (8)	C9—C10—H10B	109.5
O3—Na3—O2	83.53 (7)	H10A—C10—H10B	109.5
O6^iii—Na3—O2	80.21 (7)	C9—C10—H10C	109.5
O5—Na3—O2	110.62 (7)	H10A—C10—H10C	109.5
C2—O1—Na1	117.72 (16)	H10B—C10—H10C	109.5
C2—O1—Na2	147.40 (16)	C12—C11—H11A	109.5
Na1—O1—Na2	91.34 (7)	C12—C11—H11B	109.5
C2—O1—Na2^i	100.23 (15)	H11A—C11—H11B	109.5
Na1—O1—Na2^i	89.38 (7)	C12—C11—H11C	109.5
Na2—O1—Na2^i	94.15 (7)	H11A—C11—H11C	109.5
C4—O2—Na3	146.57 (16)	H11B—C11—H11C	109.5
C4—O2—Na1	117.62 (15)	O5—C12—C13	125.9 (2)
Na3—O2—Na1	93.56 (7)	O5—C12—C11	116.9 (2)
C4—O2—Na2^i	99.74 (15)	C13—C12—C11	117.2 (2)
Na3—O2—Na2^i	92.98 (7)	C14—C13—C12	126.8 (2)
Na1—O2—Na2^i	87.49 (7)	C14—C13—H13	116.6
C7—O3—Na1	124.09 (16)	C12—C13—H13	116.6
C7—O3—Na3	137.56 (17)	O6—C14—C13	125.5 (2)
Na1—O3—Na3	97.83 (7)	O6—C14—C15	116.2 (2)
C9—O4—Na1	124.35 (16)	C13—C14—C15	118.3 (2)
C9—O4—Na2	143.65 (18)	C14—C15—H15A	109.5
Na1—O4—Na2	90.92 (7)	C14—C15—H15B	109.5
C12—O5—Na3^iii	131.51 (16)	H15A—C15—H15B	109.5
C12—O5—Na3	127.67 (15)	C14—C15—H15C	109.5
Na3^iii—O5—Na3	94.80 (7)	H15A—C15—H15C	109.5
C14—O6—Na2^iv	126.36 (16)	H15B—C15—H15C	109.5
C14—O6—Na3^iii	130.94 (16)	N1—C16—C17	123.9 (3)
Na2^iv—O6—Na3^iii	98.88 (7)	N1—C16—H16	118.1
C20—N1—C16	116.4 (2)	C17—C16—H16	118.1
C20—N1—Na1	118.33 (19)	C16—C17—C18	118.7 (3)
C16—N1—Na1	124.82 (18)	C16—C17—H17	120.7
C2—C1—H1A	109.5	C18—C17—H17	120.7
C2—C1—H1B	109.5	C19—C18—C17	118.7 (3)
H1A—C1—H1B	109.5	C19—C18—H18	120.6
C2—C1—H1C	109.5	C17—C18—H18	120.6
H1A—C1—H1C	109.5	C18—C19—C20	118.7 (3)
H1B—C1—H1C	109.5	C18—C19—H19	120.6
O1—C2—C3	124.5 (2)	C20—C19—H19	120.6
O1—C2—C1	116.6 (2)	N1—C20—C19	123.6 (3)
C3—C2—C1	118.9 (2)	N1—C20—H20	118.2
C2—C3—C4	125.7 (2)	C19—C20—H20	118.2
C2—C3—H3	117.1

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