Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The title compound, {[Ba(H2O)6](C6H6NO)2}n, crystallizes with polymeric chains of water-bridged Ba2+ cations having additional terminally bound water mol­ecules, such that each ion is nine-coordinate. Ba and two independent water mol­ecules lie on a crystallographic mirror plane. The 6-methyl­pyridin-2-olate anions are hydrogen bonded to the cationic chains, with both O and N atoms acting as acceptors. Further O—H...O hydrogen bonding between adjacent chains results in the formation of thick sheets parallel to the ac plane; there are no significant inter­actions between these sheets.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807013037/lh2341sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807013037/lh2341Isup2.hkl
Contains datablock I

CCDC reference: 643657

Key indicators

  • Single-crystal synchrotron study
  • T = 120 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.044
  • wR factor = 0.105
  • Data-to-parameter ratio = 22.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT309_ALERT_2_C Single Bonded Oxygen (C-O .GT. 1.3 Ang) ........ O1 PLAT417_ALERT_2_C Short Inter D-H..H-D H3OB .. H2O .. 2.11 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4 PLAT736_ALERT_1_C H...A Calc 1.89(5), Rep 1.88(2) ...... 2.50 su-Ra H3# -O1 1.555 1.555 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 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 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXTL (Sheldrick, 2001); molecular graphics: DIAMOND (Brandenburg & Putz, 2004); software used to prepare material for publication: SHELXTL, publCIF (Westrip, 2007) and local programs.

catena-poly[[tri-µ-aqua-triaquabarium(II)] bis(6-methylpyridin-2-olate)] top
Crystal data top
[Ba(H2O)6](C6H6NO)2F(000) = 920
Mr = 461.67Dx = 1.696 Mg m3
Orthorhombic, PnmaSynchrotron radiation, λ = 0.6751 Å
Hall symbol: -P 2ac 2nCell parameters from 6905 reflections
a = 7.6080 (9) Åθ = 3.5–29.1°
b = 30.353 (3) ŵ = 2.24 mm1
c = 7.828 (1) ÅT = 120 K
V = 1807.7 (4) Å3Block, colourless
Z = 40.18 × 0.14 × 0.10 mm
Data collection top
Bruker APEX II CCD
diffractometer
2834 independent reflections
Radiation source: Daresbury SRS station 9.82513 reflections with I > 2σ(I)
Silicon 111 monochromatorRint = 0.039
Thin–slice ω scansθmax = 29.2°, θmin = 3.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 1010
Tmin = 0.689, Tmax = 0.807k = 4340
13751 measured reflectionsl = 1111
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)] = 0.044Hydrogen site location: difference Fourier map
wR(F2) = 0.105H atoms treated by a mixture of independent and constrained refinement
S = 1.22 w = 1/[σ2(Fo2) + (0.0225P)2 + 12.2343P]
where P = (Fo2 + 2Fc2)/3
2834 reflections(Δ/σ)max = 0.001
128 parametersΔρmax = 2.84 e Å3
8 restraintsΔρmin = 2.91 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
Ba0.53740 (5)0.25000.11370 (4)0.01415 (10)
O11.0231 (4)0.16785 (10)0.0562 (4)0.0194 (6)
O20.7751 (7)0.25000.1473 (6)0.0276 (10)
H2O0.808 (8)0.2717 (13)0.198 (7)0.033*
O30.4537 (6)0.18705 (12)0.1176 (5)0.0356 (9)
H3OA0.394 (8)0.1664 (16)0.087 (8)0.043*
H3OB0.494 (8)0.182 (2)0.213 (5)0.043*
O40.8119 (4)0.18951 (10)0.2079 (4)0.0193 (6)
H4OA0.868 (7)0.1814 (17)0.124 (5)0.023*
H4OB0.796 (7)0.1706 (18)0.269 (6)0.023*
O50.6598 (6)0.25000.4516 (5)0.0169 (8)
H5O0.632 (7)0.2720 (12)0.499 (6)0.020*
N11.2377 (5)0.12034 (12)0.0322 (4)0.0192 (7)
C11.0820 (6)0.12755 (13)0.0475 (5)0.0173 (7)
C20.9888 (6)0.09184 (14)0.1222 (5)0.0224 (8)
H20.87950.09680.17790.027*
C31.0581 (7)0.05007 (15)0.1132 (6)0.0261 (9)
H30.99680.02600.16290.031*
C41.2186 (7)0.04304 (14)0.0312 (6)0.0255 (9)
H41.26770.01430.02440.031*
C51.3048 (6)0.07880 (14)0.0402 (5)0.0217 (8)
C61.4797 (7)0.07435 (18)0.1274 (7)0.0335 (11)
H6A1.56420.09460.07460.050*
H6B1.52210.04400.11560.050*
H6C1.46710.08150.24880.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba0.01499 (16)0.01746 (15)0.01001 (14)0.0000.00016 (12)0.000
O10.0228 (15)0.0205 (13)0.0147 (12)0.0004 (12)0.0006 (12)0.0016 (10)
O20.032 (3)0.028 (2)0.023 (2)0.0000.010 (2)0.000
O30.046 (2)0.0329 (18)0.0276 (17)0.0hydrogen179 (17)0.0187 (17)0.0137 (14)
O40.0232 (16)0.0196 (13)0.0151 (13)0.0016 (12)0.0031 (11)0.0012 (10)
O50.019 (2)0.0198 (19)0.0123 (17)0.0000.0013 (15)0.000
N10.0231 (18)0.0193 (16)0.0153 (15)0.0004 (14)0.0013 (13)0.0010 (12)
C10.021 (2)0.0210 (18)0.0105 (15)0.0015 (14)0.0021 (13)0.0003 (13)
C20.023 (2)0.0246 (19)0.0194 (18)0.0045 (16)0.0041 (15)0.0001 (15)
C30.034 (3)0.0218 (19)0.0223 (19)0.0079 (17)0.0003 (19)0.0020 (16)
C40.035 (3)0.0182 (19)0.024 (2)0.0018 (17)0.0040 (18)0.0007 (15)
C50.024 (2)0.025 (2)0.0158 (17)0.0015 (17)0.0024 (16)0.0011 (14)
C60.032 (3)0.034 (2)0.034 (3)0.008 (2)0.007 (2)0.002 (2)
Geometric parameters (Å, º) top
Ba—O22.729 (5)O5—Baiv2.918 (4)
Ba—O32.708 (3)O5—H5O0.79 (3)
Ba—O3i2.708 (3)N1—C11.357 (5)
Ba—O42.877 (3)N1—C51.362 (5)
Ba—O4ii2.875 (3)C1—C21.421 (6)
Ba—O4iii2.875 (3)C2—H20.9500
Ba—O4i2.877 (3)C2—C31.375 (6)
Ba—O52.804 (4)C3—H30.950
Ba—O5iii2.918 (4)C3—C41.396 (7)
O1—C11.305 (5)C4—H40.950
O2—H2O0.81 (3)C4—C51.386 (6)
O3—H3OA0.81 (3)C5—C61.501 (7)
O3—H3OB0.82 (3)C6—H6A0.980
O4—Baiv2.875 (3)C6—H6B0.980
O4—H4OA0.82 (2)C6—H6C0.980
O4—H4OB0.76 (5)
O2—Ba—O369.83 (11)Ba—O2—H2O125 (4)
O2—Ba—O3i69.83 (11)Ba—O3—H3OA119 (4)
O2—Ba—O473.18 (11)Ba—O3—H3OB131 (4)
O2—Ba—O4ii139.41 (6)H3OA—O3—H3OB109 (5)
O2—Ba—O4iii139.40 (6)Ba—O4—Baiv98.63 (9)
O2—Ba—O4i73.18 (11)Ba—O4—H4OA111 (4)
O2—Ba—O5119.09 (15)Baiv—O4—H4OA105 (4)
O2—Ba—O5iii121.43 (14)Ba—O4—H4OB122 (4)
O3—Ba—O3i89.75 (19)Baiv—O4—H4OB106 (4)
O3—Ba—O483.78 (12)H4OA—O4—H4OB111 (5)
O3—Ba—O4ii129.43 (12)Ba—O5—Baiv99.30 (13)
O3i—Ba—O4ii74.57 (10)Ba—O5—H5O111 (4)
O3—Ba—O4iii74.57 (10)Baiv—O5—H5O110 (4)
O3i—Ba—O4iii129.43 (12)C1—N1—C5119.9 (4)
O3—Ba—O4i142.40 (10)O1—C1—N1118.4 (4)
O3i—Ba—O4i83.78 (12)O1—C1—C2121.5 (4)
O3i—Ba—O4142.40 (10)N1—C1—C2120.1 (4)
O3—Ba—O5135.12 (9)C1—C2—H2120.3
O3i—Ba—O5135.12 (9)C1—C2—C3119.4 (4)
O3—Ba—O5iii69.60 (11)H2—C2—C3120.3
O3i—Ba—O5iii69.60 (11)C2—C3—H3120.0
O4ii—Ba—O4iii79.38 (12)C2—C3—C4120.0 (4)
O4ii—Ba—O4i84.33 (7)H3—C3—C4120.0
O4iii—Ba—O4i135.75 (4)C3—C4—H4120.7
O4—Ba—O4ii135.75 (4)C3—C4—C5118.7 (4)
O4—Ba—O4iii84.33 (7)H4—C4—C5120.7
O4—Ba—O4i79.32 (13)N1—C5—C4121.9 (4)
O4—Ba—O561.13 (8)N1—C5—C6115.9 (4)
O4ii—Ba—O574.93 (9)C4—C5—C6122.2 (4)
O4iii—Ba—O574.93 (9)C5—C6—H6A109.5
O4i—Ba—O561.13 (8)C5—C6—H6B109.5
O4ii—Ba—O5iii59.84 (8)C5—C6—H6C109.5
O4iii—Ba—O5iii59.84 (8)H6A—C6—H6B109.5
O4i—Ba—O5iii139.43 (7)H6A—C6—H6C109.5
O4—Ba—O5iii139.43 (7)H6B—C6—H6C109.5
O5—Ba—O5iii119.48 (11)
O2—Ba—O4—Baiv90.70 (11)O4i—Ba—O5—Baiv46.79 (8)
O3—Ba—O4—Baiv161.47 (11)O4—Ba—O5—Baiv46.79 (8)
O3i—Ba—O4—Baiv80.03 (19)O5iii—Ba—O5—Baiv180.0
O4ii—Ba—O4—Baiv55.05 (15)C5—N1—C1—O1178.6 (4)
O4iii—Ba—O4—Baiv123.49 (13)C5—N1—C1—C20.2 (6)
O4i—Ba—O4—Baiv15.21 (12)O1—C1—C2—C3178.5 (4)
O5—Ba—O4—Baiv47.59 (9)N1—C1—C2—C30.2 (6)
O5iii—Ba—O4—Baiv150.31 (13)C1—C2—C3—C40.1 (7)
Baiii—Ba—O5—Baiv180.0C2—C3—C4—C50.1 (7)
O2—Ba—O5—Baiv0.0C1—N1—C5—C40.0 (6)
O3—Ba—O5—Baiv89.98 (15)C1—N1—C5—C6178.6 (4)
O3i—Ba—O5—Baiv89.98 (15)C3—C4—C5—N10.1 (7)
O4ii—Ba—O5—Baiv138.59 (6)C3—C4—C5—C6178.6 (4)
O4iii—Ba—O5—Baiv138.59 (6)
Symmetry codes: (i) x, y+1/2, z; (ii) x1/2, y+1/2, z+1/2; (iii) x1/2, y, z+1/2; (iv) x+1/2, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H2O···O3v0.81 (3)2.21 (3)2.981 (6)160 (6)
O3—H3OA···N1vi0.81 (3)2.06 (3)2.859 (5)170 (6)
O3—H3OB···O1vii0.82 (3)1.87 (3)2.672 (5)165 (6)
O4—H4OA···O10.82 (2)1.88 (2)2.699 (4)172 (6)
O4—H4OB···N1iii0.76 (5)2.23 (5)2.977 (5)174 (5)
O5—H5O···O1ii0.79 (3)2.06 (3)2.823 (4)163 (5)
Symmetry codes: (ii) x1/2, y+1/2, z+1/2; (iii) x1/2, y, z+1/2; (v) x+1/2, y+1/2, z1/2; (vi) x1, y, z; (vii) x1/2, y, z1/2.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds