metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 2| February 2011| Pages m283-m284

Poly[[hepta-μ2-aqua-bis­­(μ2-pyrazine-2-carboxyl­ato)dibarium] bis­­(pyrazine-2-carboxyl­ate)]

aCollege of Science, Northwest A&F University, Yangling 712100, Shanxi Province, People's Republic of China, and bStudents Service, Northwest A&F University, Yangling 712100, Shanxi Province, People's Republic of China
*Correspondence e-mail: shuaiqi@nwsuaf.edu.cn

(Received 5 December 2010; accepted 23 January 2011; online 29 January 2011)

In the layered title coordination polymer, {[Ba2(C5H3N2O2)2(H2O)7](C5H3N2O2)2}n, the coordination geometries around the two independent BaII ions can be described as bicapped square-anti­prismatic [BaNO9] arrangements. A two-dimensional polymeric framework with (6,3) topology can be observed in the ac plane, the nodes being provided by BaII ions and the connectors being N and O atoms belonging to pyrazine-2-carboxyl­ate ligands and O atoms of bridging water mol­ecules. Non-coordinating pyrazine-2-carboxyl­ate ions are located between the polymeric layers in the crystal and are interconnected through extensive O—H⋯N,O hydrogen bonding.

Related literature

For CaII and SrII complexes with pyrazine-2-carboxyl­ate as ligand, see: Ptasiewicz-Bak et al. (1998[Ptasiewicz-Bak, H., Ostrowski, A. & Leciejewicz, J. (1998). Pol. J. Chem. 72, 2014-2023.]). For different modes of coordination for pyrazine-2-carboxyl­ate in polymers, see: Huang et al. (2003[Huang, D., Zhang, X., Chen, C., Chen, F., Liu, Q., Liao, D., Li, L. & Sun, L. (2003). Inorg. Chim. Acta, 353, 284-291.]); Yin et al. (2006[Yin, H. D., Li, G., Gao, Z. J. & Xu, H. L. (2006). J. Organomet. Chem. 691, 1235-1241.]).

[Scheme 1]

Experimental

Crystal data
  • [Ba2(C5H3N2O2)2(H2O)7](C5H3N2O2)2

  • Mr = 893.17

  • Monoclinic, P 21

  • a = 7.5652 (10) Å

  • b = 29.263 (3) Å

  • c = 7.6067 (10) Å

  • β = 118.741 (2)°

  • V = 1476.5 (3) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 2.74 mm−1

  • T = 298 K

  • 0.49 × 0.34 × 0.16 mm

Data collection
  • Bruker SMART APEX CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2002[Bruker (2002). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.348, Tmax = 0.669

  • 7342 measured reflections

  • 4734 independent reflections

  • 4502 reflections with I > 2σ(I)

  • Rint = 0.036

Refinement
  • R[F2 > 2σ(F2)] = 0.046

  • wR(F2) = 0.121

  • S = 1.02

  • 4734 reflections

  • 406 parameters

  • 1 restraint

  • H-atom parameters constrained

  • Δρmax = 1.84 e Å−3

  • Δρmin = −2.62 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 2096 Friedel pairs

  • Flack parameter: 0.04 (4)

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O10—H10A⋯O7 0.85 2.23 3.000 (13) 152
O10—H10B⋯O5 0.85 1.92 2.769 (11) 177
O11—H11A⋯O4 0.85 1.88 2.669 (12) 153
O11—H11B⋯O5 0.85 2.04 2.861 (12) 163
O11—H11B⋯N5 0.85 2.62 3.191 (14) 126
O13—H13A⋯N5 0.85 2.14 2.983 (14) 175
O14—H14A⋯O8 0.85 1.87 2.685 (12) 160
O9—H9A⋯O7i 0.85 1.88 2.677 (12) 155
O9—H9B⋯O5i 0.85 1.89 2.689 (12) 156
O13—H13B⋯O6i 0.85 1.93 2.729 (12) 157
O15—H15A⋯O7i 0.85 2.04 2.860 (12) 161
O15—H15A⋯N7i 0.85 2.62 3.208 (14) 127
O12—H12A⋯O7ii 0.85 1.96 2.811 (12) 179
O12—H12B⋯O5ii 0.85 2.26 3.018 (12) 149
O14—H14B⋯N7ii 0.85 2.18 3.028 (13) 174
O15—H15B⋯O2iii 0.85 1.90 2.676 (11) 152
Symmetry codes: (i) x+1, y, z; (ii) x, y, z-1; (iii) x, y, z+1.

Data collection: SMART (Bruker, 2002[Bruker (2002). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2002[Bruker (2002). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

Ptasiewicz-Bak et al. obtained monomeric complexes of calcium and strontium [M(C5H3N2O2)2(H2O)4] (M = CaII or SrII, Ptasiewicz-Bak et al., 1998), based on 2-pyrazinecarboxylate ligand, which are isostructural.

Here, we report a complex, (I), assembled by alkaline earth metal BaII ion with 2-pyrazinecarboxylate as ligand. Different from complexes of calcium and strontium, the formula for the title complex is [Ba2(C5H3N2O2)2(H2O)7] (C5H3N2O2)2. X-ray single-crystal diffraction analysis indicates the presence of two independent BaII ions, two coordinated pyrazine-2-carboxylate ions, seven coordinated water molecules and two isolated pyrazine-2-carboxylate ions in the asymmetric unit. Only one independent CaII or SrII ions are found in the complexes reported by Ptasiewicz-Bak et al.

In the title complex, the coordination geometries (Fig. 1) around Ba1 and Ba2 centres could be described as bicapped square-antiprismatic [BaNO9] arrangements with coordination number of 10, where one N and two O atoms come from 2-pyrazinecarboxylate ligands, the rest, seven O atoms, being from seven coordinated water molecules. There are two kinds of pyrizine-2-carboxylate coordination modes, which have been reported previously (Yin et al., 2006; Huang et al., 2003). In (I), only one kind of coordination mode, µ2 bridging mode, is observed. All the water molecules are coordinated and act as µ2 bridging ligands. In this case, every six BaII ions form metal hexameric rings which share common edges, to construct two-dimensional, infinite networks with (6,3) topology (Fig. 2) parallel to the ac plane. Within the (6,3) topology layer, the nodes are provided by BaII and the connectors are N and O atoms which come from 2-pyrazinecarboxylate ions, and O atoms of water molecules. Non coordinating pyrazine-2-carboxylate ions are placed between polymeric layers in the crystal.

Related literature top

For CaII and SrII complexes with pyrazine-2-carboxylate as ligand, see: Ptasiewicz-Bak et al. (1998). For different modes of coordination for pyrazine-2-carboxylate in polymers, see: Huang et al. (2003); Yin et al. (2006).

Experimental top

A mixture of barium chloride dihydrate (0.0244 g, 0.1 mmol), sodium hydroxide (0.0160 g, 0.4 mmol), 2-pyrazinecarboxylic acid (0.0496 g, 0.4 mmol), and H2O (3 ml) was placed in a Parr Teflon-lined stainless steel vessel (25 ml). The vessel was sealed and heated to 443.15 K for 6 days. Then, the vessel was cooled to 373.15 K at a rate of 5 K.h-1 and slowly cooled to room temperature. Colourless, rectangular single crystals suitable for X-ray diffraction were obtained.

Refinement top

All H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms, with aromatic C—H = 0.93 Å, O—H = 0.85 Å and refined as riding on their parent atoms. TheUiso(H) values were set at 1.2Ueq(carrier atom) for all H atoms.

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Coordination environment of BaII ions in the title complex. Non-hydrogen atoms are shown as 30% probability ellipsoids. Hydrogen atoms are omitted for clarity.
[Figure 2] Fig. 2. View of one two-dimensional layer structure along b axis in the title complex. Hydrogen atoms are omitted for clarity. Some redundant atoms are omitted for clarity.
Poly[[hepta-µ2-aqua-bis(µ2-pyrazine-2-carboxylato)dibarium] bis(pyrazine-2-carboxylate)] top
Crystal data top
[Ba2(C5H3N2O2)2(H2O)7](C5H3N2O2)2F(000) = 868
Mr = 893.17Dx = 2.009 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ybCell parameters from 4314 reflections
a = 7.5652 (10) Åθ = 2.8–27.6°
b = 29.263 (3) ŵ = 2.74 mm1
c = 7.6067 (10) ÅT = 298 K
β = 118.741 (2)°Block, colourless
V = 1476.5 (3) Å30.49 × 0.34 × 0.16 mm
Z = 2
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
4734 independent reflections
Radiation source: fine-focus sealed tube4502 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
Detector resolution: 0 pixels mm-1θmax = 25.0°, θmin = 1.4°
ϕ and ω scansh = 86
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
k = 3432
Tmin = 0.348, Tmax = 0.669l = 89
7342 measured reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.046 w = 1/[σ2(Fo2) + (0.062P)2 + 10.4333P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.121(Δ/σ)max < 0.001
S = 1.02Δρmax = 1.84 e Å3
4734 reflectionsΔρmin = 2.62 e Å3
406 parametersExtinction correction: SHELXL97 (Sheldrick, 2008)
1 restraintExtinction coefficient: 0.00273 (13)
0 constraintsAbsolute structure: Flack (1983), 2096 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.04 (4)
Secondary atom site location: difference Fourier map
Crystal data top
[Ba2(C5H3N2O2)2(H2O)7](C5H3N2O2)2V = 1476.5 (3) Å3
Mr = 893.17Z = 2
Monoclinic, P21Mo Kα radiation
a = 7.5652 (10) ŵ = 2.74 mm1
b = 29.263 (3) ÅT = 298 K
c = 7.6067 (10) Å0.49 × 0.34 × 0.16 mm
β = 118.741 (2)°
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
4734 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
4502 reflections with I > 2σ(I)
Tmin = 0.348, Tmax = 0.669Rint = 0.036
7342 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.046H-atom parameters constrained
wR(F2) = 0.121 w = 1/[σ2(Fo2) + (0.062P)2 + 10.4333P]
where P = (Fo2 + 2Fc2)/3
S = 1.02Δρmax = 1.84 e Å3
4734 reflectionsΔρmin = 2.62 e Å3
406 parametersAbsolute structure: Flack (1983), 2096 Friedel pairs
1 restraintAbsolute structure parameter: 0.04 (4)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.77811 (9)0.366622 (19)0.36016 (9)0.02014 (17)
Ba21.10429 (9)0.394536 (18)0.03210 (9)0.01982 (16)
N10.8301 (16)0.2639 (3)0.3451 (15)0.026 (2)
N20.888 (2)0.1707 (4)0.308 (2)0.043 (3)
N31.0849 (15)0.4975 (4)0.0828 (17)0.028 (2)
N41.045 (2)0.5910 (4)0.137 (2)0.045 (3)
N50.6725 (18)0.5151 (4)0.6133 (18)0.033 (3)
N60.5658 (18)0.6073 (4)0.610 (2)0.039 (3)
N70.3586 (18)0.2445 (4)0.9189 (19)0.032 (3)
N80.400 (2)0.1538 (4)0.828 (2)0.052 (4)
O10.8792 (14)0.3243 (3)0.0951 (15)0.034 (2)
O20.9048 (17)0.2671 (3)0.0797 (14)0.039 (2)
O30.8422 (13)0.4370 (3)0.1352 (14)0.033 (2)
O40.6620 (16)0.4940 (3)0.1590 (18)0.045 (3)
O50.4326 (14)0.4487 (3)0.6353 (16)0.040 (2)
O60.2265 (14)0.5026 (4)0.6485 (15)0.043 (3)
O70.3818 (16)0.3133 (3)0.6871 (15)0.042 (2)
O80.4035 (18)0.2619 (4)0.4835 (15)0.051 (3)
O91.1777 (11)0.3806 (3)0.4331 (11)0.0267 (17)
H9A1.25150.35730.48650.032*
H9B1.23120.40400.50610.032*
O100.6963 (12)0.3775 (3)0.6959 (12)0.0278 (18)
H10A0.64500.35340.71490.033*
H10B0.61820.40000.67770.033*
O110.4867 (12)0.4342 (3)0.2934 (13)0.0288 (19)
H11A0.50660.45770.23960.035*
H11B0.49210.44210.40350.035*
O120.4417 (12)0.3857 (3)0.0462 (12)0.031 (2)
H12A0.42410.36370.12590.038*
H12B0.46140.41020.09450.038*
O130.9582 (12)0.4406 (3)0.6526 (12)0.0294 (18)
H13A0.87060.46070.63720.035*
H13B1.05410.45330.64260.035*
O140.3952 (12)0.3203 (3)0.2065 (13)0.0296 (19)
H14A0.38380.30710.30010.036*
H14B0.38060.30060.11820.036*
O151.0377 (12)0.3263 (3)0.7417 (12)0.0271 (18)
H15A1.14860.31820.74810.032*
H15B0.98230.30290.76080.032*
C10.8864 (17)0.2828 (4)0.0620 (17)0.021 (2)
C20.874 (2)0.2485 (4)0.2049 (19)0.027 (3)
C30.896 (2)0.2017 (4)0.184 (2)0.036 (3)
H30.91710.19180.07900.043*
C50.847 (3)0.1868 (6)0.449 (3)0.046 (4)
H50.83600.16660.53730.056*
C60.822 (2)0.2336 (5)0.467 (2)0.036 (3)
H60.79790.24350.56950.043*
C70.804 (2)0.4782 (5)0.1384 (19)0.030 (3)
C80.944 (2)0.5124 (4)0.1270 (19)0.030 (3)
C90.923 (2)0.5590 (5)0.149 (2)0.039 (3)
H90.81930.56850.17360.047*
C111.187 (2)0.5754 (5)0.100 (3)0.041 (4)
H111.27680.59600.09320.050*
C121.207 (2)0.5296 (5)0.071 (2)0.034 (3)
H121.30880.52050.04320.041*
C130.3801 (19)0.4890 (4)0.640 (2)0.026 (3)
C140.5088 (18)0.5268 (4)0.6264 (17)0.022 (2)
C150.461 (2)0.5730 (5)0.624 (2)0.036 (3)
H150.34580.58010.63410.043*
C170.727 (2)0.5944 (5)0.592 (2)0.036 (3)
H170.80580.61680.57710.043*
C180.779 (2)0.5490 (5)0.595 (2)0.041 (4)
H180.89320.54190.58400.049*
C190.396 (2)0.2731 (4)0.636 (2)0.028 (3)
C200.3868 (17)0.2347 (4)0.7658 (19)0.026 (3)
C210.409 (2)0.1888 (5)0.723 (2)0.038 (3)
H210.43210.18280.61590.045*
C230.363 (2)0.1655 (6)0.977 (2)0.045 (4)
H230.34940.14241.05330.054*
C240.346 (2)0.2099 (5)1.022 (2)0.043 (4)
H240.32320.21591.12960.051*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba10.0175 (3)0.0207 (3)0.0234 (3)0.0000 (3)0.0108 (3)0.0010 (3)
Ba20.0184 (3)0.0207 (3)0.0216 (3)0.0006 (3)0.0106 (3)0.0005 (3)
N10.036 (6)0.013 (5)0.030 (6)0.005 (4)0.017 (5)0.003 (4)
N20.053 (8)0.023 (6)0.065 (8)0.011 (5)0.038 (7)0.007 (6)
N30.029 (6)0.029 (6)0.041 (6)0.006 (5)0.029 (5)0.011 (5)
N40.053 (8)0.019 (6)0.073 (9)0.005 (5)0.039 (7)0.001 (6)
N50.028 (6)0.032 (6)0.042 (7)0.000 (5)0.018 (5)0.005 (5)
N60.042 (7)0.015 (6)0.065 (9)0.006 (5)0.028 (6)0.002 (5)
N70.036 (6)0.029 (6)0.038 (6)0.005 (5)0.025 (6)0.006 (5)
N80.096 (11)0.018 (6)0.049 (8)0.005 (6)0.041 (8)0.007 (6)
O10.042 (5)0.019 (5)0.053 (6)0.002 (4)0.031 (5)0.001 (4)
O20.076 (7)0.021 (5)0.036 (5)0.003 (5)0.042 (6)0.001 (4)
O30.040 (5)0.022 (5)0.055 (6)0.006 (4)0.037 (5)0.010 (4)
O40.047 (6)0.028 (5)0.082 (8)0.007 (4)0.049 (6)0.007 (5)
O50.043 (6)0.030 (5)0.060 (6)0.002 (4)0.034 (5)0.008 (5)
O60.043 (6)0.035 (6)0.070 (8)0.003 (4)0.042 (6)0.001 (5)
O70.052 (6)0.037 (5)0.046 (6)0.013 (5)0.031 (5)0.001 (5)
O80.092 (9)0.038 (6)0.042 (6)0.002 (6)0.047 (7)0.006 (5)
O90.020 (4)0.033 (4)0.025 (4)0.000 (3)0.008 (3)0.004 (3)
O100.028 (4)0.027 (5)0.036 (4)0.000 (3)0.022 (4)0.001 (4)
O110.023 (4)0.027 (5)0.039 (5)0.004 (3)0.017 (4)0.008 (4)
O120.041 (5)0.031 (5)0.030 (4)0.006 (4)0.024 (4)0.002 (4)
O130.028 (4)0.025 (4)0.041 (5)0.000 (3)0.021 (4)0.000 (4)
O140.037 (5)0.016 (4)0.041 (5)0.004 (3)0.023 (4)0.002 (4)
O150.031 (5)0.020 (4)0.031 (5)0.003 (3)0.016 (4)0.002 (3)
C10.020 (6)0.027 (7)0.018 (6)0.009 (5)0.011 (5)0.002 (5)
C20.041 (8)0.021 (6)0.028 (7)0.009 (5)0.024 (6)0.008 (5)
C30.070 (10)0.007 (6)0.058 (9)0.001 (6)0.052 (9)0.002 (6)
C50.049 (9)0.037 (9)0.055 (10)0.001 (8)0.027 (8)0.014 (8)
C60.045 (8)0.041 (8)0.023 (7)0.004 (7)0.018 (6)0.005 (6)
C70.033 (7)0.030 (7)0.032 (7)0.004 (6)0.020 (6)0.006 (6)
C80.042 (8)0.017 (6)0.029 (7)0.000 (5)0.016 (6)0.001 (5)
C90.049 (9)0.033 (8)0.049 (9)0.002 (6)0.035 (8)0.003 (6)
C110.040 (8)0.029 (8)0.059 (10)0.006 (7)0.027 (8)0.013 (7)
C120.032 (7)0.042 (8)0.035 (8)0.004 (6)0.021 (6)0.002 (6)
C130.024 (6)0.029 (7)0.030 (7)0.009 (5)0.016 (6)0.008 (5)
C140.028 (6)0.016 (6)0.024 (6)0.002 (5)0.015 (5)0.001 (5)
C150.044 (8)0.027 (7)0.048 (9)0.004 (6)0.033 (7)0.001 (6)
C170.043 (8)0.021 (7)0.049 (9)0.008 (6)0.027 (7)0.006 (6)
C180.032 (7)0.039 (8)0.063 (10)0.011 (6)0.031 (8)0.003 (7)
C190.037 (7)0.029 (7)0.025 (7)0.007 (5)0.020 (6)0.003 (5)
C200.018 (6)0.025 (7)0.035 (7)0.004 (5)0.011 (5)0.000 (5)
C210.053 (9)0.025 (7)0.039 (8)0.003 (6)0.025 (7)0.005 (6)
C230.056 (10)0.042 (9)0.034 (8)0.003 (7)0.019 (8)0.010 (7)
C240.043 (9)0.054 (10)0.037 (8)0.000 (7)0.024 (7)0.006 (7)
Geometric parameters (Å, º) top
Ba1—O12.769 (9)O9—H9A0.8500
Ba1—O112.821 (8)O9—H9B0.8500
Ba1—O92.829 (7)O10—Ba2iii2.954 (8)
Ba1—O152.862 (8)O10—H10A0.8500
Ba1—O32.865 (8)O10—H10B0.8501
Ba1—O142.888 (8)O11—Ba2iv2.853 (8)
Ba1—O102.920 (7)O11—H11A0.8499
Ba1—O132.930 (8)O11—H11B0.8500
Ba1—O122.963 (8)O12—Ba2iv2.898 (8)
Ba1—N13.041 (10)O12—H12A0.8499
Ba2—O32.754 (8)O12—H12B0.8501
Ba2—O15i2.838 (8)O13—Ba2iii2.882 (8)
Ba2—O11ii2.853 (8)O13—H13A0.8499
Ba2—O12.853 (8)O13—H13B0.8499
Ba2—O92.854 (7)O14—Ba2iv2.919 (8)
Ba2—O13i2.882 (8)O14—H14A0.8499
Ba2—O12ii2.898 (8)O14—H14B0.8501
Ba2—O14ii2.919 (8)O15—Ba2iii2.838 (8)
Ba2—O10i2.954 (8)O15—H15A0.8500
Ba2—N33.050 (11)O15—H15B0.8501
N1—C61.305 (17)C1—C21.515 (16)
N1—C21.336 (16)C2—C31.401 (17)
N2—C31.332 (17)C3—H30.9300
N2—C51.34 (2)C5—C61.40 (2)
N3—C81.334 (17)C5—H50.9300
N3—C121.351 (17)C6—H60.9300
N4—C111.32 (2)C7—C81.489 (18)
N4—C91.349 (18)C8—C91.394 (19)
N5—C181.326 (18)C9—H90.9300
N5—C141.334 (16)C11—C121.38 (2)
N6—C151.317 (17)C11—H110.9300
N6—C171.341 (18)C12—H120.9300
N7—C241.312 (19)C13—C141.509 (16)
N7—C201.313 (16)C14—C151.400 (18)
N8—C211.320 (18)C15—H150.9300
N8—C231.331 (19)C17—C181.39 (2)
O1—C11.246 (14)C17—H170.9300
O2—C11.240 (14)C18—H180.9300
O3—C71.243 (15)C19—C201.519 (18)
O4—C71.248 (16)C20—C211.413 (19)
O5—C131.249 (15)C21—H210.9300
O6—C131.259 (15)C23—C241.37 (2)
O7—C191.260 (16)C23—H230.9300
O8—C191.233 (15)C24—H240.9300
O1—Ba1—O11130.4 (3)O13i—Ba2—Ba1ii115.01 (16)
O1—Ba1—O964.2 (2)O12ii—Ba2—Ba1ii39.69 (16)
O11—Ba1—O9127.1 (2)O14ii—Ba2—Ba1ii38.27 (16)
O1—Ba1—O15105.0 (2)O10i—Ba2—Ba1ii150.97 (15)
O11—Ba1—O15124.6 (2)N3—Ba2—Ba1ii102.6 (2)
O9—Ba1—O1573.3 (2)Ba1—Ba2—Ba1ii116.58 (2)
O1—Ba1—O372.6 (2)C6—N1—C2116.8 (11)
O11—Ba1—O374.4 (2)C6—N1—Ba1126.5 (9)
O9—Ba1—O362.7 (2)C2—N1—Ba1116.6 (8)
O15—Ba1—O3132.2 (3)C3—N2—C5115.8 (12)
O1—Ba1—O1494.0 (2)C8—N3—C12116.4 (12)
O11—Ba1—O1473.3 (2)C8—N3—Ba2116.6 (8)
O9—Ba1—O14156.4 (2)C12—N3—Ba2127.0 (8)
O15—Ba1—O14106.4 (2)C11—N4—C9115.5 (12)
O3—Ba1—O14121.4 (3)C18—N5—C14116.8 (13)
O1—Ba1—O10159.1 (2)C15—N6—C17114.2 (11)
O11—Ba1—O1066.7 (2)C24—N7—C20116.9 (13)
O9—Ba1—O10118.0 (2)C21—N8—C23114.0 (13)
O15—Ba1—O1059.2 (2)C1—O1—Ba1129.6 (7)
O3—Ba1—O10127.8 (2)C1—O1—Ba2125.5 (7)
O14—Ba1—O1079.2 (2)Ba1—O1—Ba2101.3 (3)
O1—Ba1—O13133.9 (2)C7—O3—Ba2130.5 (8)
O11—Ba1—O1369.9 (2)C7—O3—Ba1125.3 (8)
O9—Ba1—O1371.4 (2)Ba2—O3—Ba1101.4 (3)
O15—Ba1—O1372.1 (2)Ba1—O9—Ba299.8 (2)
O3—Ba1—O1376.8 (2)Ba1—O9—H9A111.8
O14—Ba1—O13131.6 (2)Ba2—O9—H9A111.8
O10—Ba1—O1358.1 (2)Ba1—O9—H9B111.8
O1—Ba1—O1274.0 (3)Ba2—O9—H9B111.8
O11—Ba1—O1258.3 (2)H9A—O9—H9B109.6
O9—Ba1—O12118.6 (2)Ba1—O10—Ba2iii101.7 (2)
O15—Ba1—O12164.2 (2)Ba1—O10—H10A111.4
O3—Ba1—O1263.1 (3)Ba2iii—O10—H10A111.4
O14—Ba1—O1258.4 (2)Ba1—O10—H10B111.4
O10—Ba1—O12117.1 (2)Ba2iii—O10—H10B111.4
O13—Ba1—O12120.4 (2)H10A—O10—H10B109.3
O1—Ba1—N156.2 (3)Ba1—O11—Ba2iv106.4 (3)
O11—Ba1—N1142.2 (3)Ba1—O11—H11A110.4
O9—Ba1—N190.3 (3)Ba2iv—O11—H11A110.4
O15—Ba1—N165.9 (2)Ba1—O11—H11B110.4
O3—Ba1—N1128.8 (3)Ba2iv—O11—H11B110.4
O14—Ba1—N169.1 (3)H11A—O11—H11B108.7
O10—Ba1—N1103.1 (3)Ba2iv—O12—Ba1101.6 (2)
O13—Ba1—N1137.6 (3)Ba2iv—O12—H12A111.2
O12—Ba1—N1102.1 (3)Ba1—O12—H12A111.2
O1—Ba1—Ba240.06 (17)Ba2iv—O12—H12B111.6
O11—Ba1—Ba2112.03 (18)Ba1—O12—H12B111.6
O9—Ba1—Ba240.31 (15)H12A—O12—H12B109.3
O15—Ba1—Ba2110.94 (17)Ba2iii—O13—Ba1103.2 (2)
O3—Ba1—Ba238.39 (16)Ba2iii—O13—H13A111.0
O14—Ba1—Ba2126.27 (17)Ba1—O13—H13A111.0
O10—Ba1—Ba2154.02 (16)Ba2iii—O13—H13B111.2
O13—Ba1—Ba296.42 (16)Ba1—O13—H13B111.1
O12—Ba1—Ba278.79 (15)H13A—O13—H13B109.2
N1—Ba1—Ba292.6 (2)Ba1—O14—Ba2iv103.0 (2)
O1—Ba1—Ba2iv108.1 (2)Ba1—O14—H14A111.1
O11—Ba1—Ba2iv37.04 (16)Ba2iv—O14—H14A111.1
O9—Ba1—Ba2iv153.20 (16)Ba1—O14—H14B111.2
O15—Ba1—Ba2iv132.27 (17)Ba2iv—O14—H14B111.2
O3—Ba1—Ba2iv90.58 (18)H14A—O14—H14B109.2
O14—Ba1—Ba2iv38.76 (15)Ba2iii—O15—Ba1106.1 (2)
O10—Ba1—Ba2iv78.88 (15)Ba2iii—O15—H15A110.5
O13—Ba1—Ba2iv105.87 (16)Ba1—O15—H15A110.5
O12—Ba1—Ba2iv38.66 (15)Ba2iii—O15—H15B110.5
N1—Ba1—Ba2iv106.8 (2)Ba1—O15—H15B110.5
Ba2—Ba1—Ba2iv116.58 (2)H15A—O15—H15B108.7
O3—Ba2—O15i131.0 (3)O2—C1—O1124.8 (11)
O3—Ba2—O11ii104.2 (2)O2—C1—C2116.8 (10)
O15i—Ba2—O11ii124.7 (2)O1—C1—C2118.4 (10)
O3—Ba2—O173.0 (2)N1—C2—C3120.7 (11)
O15i—Ba2—O174.1 (2)N1—C2—C1118.4 (11)
O11ii—Ba2—O1131.6 (3)C3—C2—C1120.8 (10)
O3—Ba2—O963.7 (2)N2—C3—C2122.4 (12)
O15i—Ba2—O9127.0 (2)N2—C3—H3118.8
O11ii—Ba2—O972.7 (2)C2—C3—H3118.8
O1—Ba2—O962.8 (3)N2—C5—C6121.3 (14)
O3—Ba2—O13i95.3 (2)N2—C5—H5119.3
O15i—Ba2—O13i73.2 (2)C6—C5—H5119.3
O11ii—Ba2—O13i106.2 (2)N1—C6—C5122.8 (13)
O1—Ba2—O13i122.2 (3)N1—C6—H6118.6
O9—Ba2—O13i157.1 (2)C5—C6—H6118.6
O3—Ba2—O12ii157.6 (2)O3—C7—O4125.7 (12)
O15i—Ba2—O12ii67.8 (2)O3—C7—C8118.2 (11)
O11ii—Ba2—O12ii58.8 (2)O4—C7—C8116.1 (12)
O1—Ba2—O12ii128.8 (2)N3—C8—C9120.3 (12)
O9—Ba2—O12ii118.0 (2)N3—C8—C7118.1 (11)
O13i—Ba2—O12ii77.7 (2)C9—C8—C7121.5 (12)
O3—Ba2—O14ii134.1 (2)N4—C9—C8123.2 (13)
O15i—Ba2—O14ii69.0 (2)N4—C9—H9118.4
O11ii—Ba2—O14ii72.3 (2)C8—C9—H9118.4
O1—Ba2—O14ii76.6 (2)N4—C11—C12122.5 (13)
O9—Ba2—O14ii72.0 (2)N4—C11—H11118.8
O13i—Ba2—O14ii130.2 (2)C12—C11—H11118.8
O12ii—Ba2—O14ii58.7 (2)N3—C12—C11122.2 (12)
O3—Ba2—O10i74.2 (2)N3—C12—H12118.9
O15i—Ba2—O10i59.1 (2)C11—C12—H12118.9
O11ii—Ba2—O10i163.6 (2)O5—C13—O6127.8 (12)
O1—Ba2—O10i64.2 (2)O5—C13—C14117.7 (11)
O9—Ba2—O10i119.1 (2)O6—C13—C14114.4 (11)
O13i—Ba2—O10i58.3 (2)N5—C14—C15119.5 (12)
O12ii—Ba2—O10i117.6 (2)N5—C14—C13118.1 (11)
O14ii—Ba2—O10i120.9 (2)C15—C14—C13122.5 (11)
O3—Ba2—N355.5 (2)N6—C15—C14124.9 (12)
O15i—Ba2—N3142.4 (3)N6—C15—H15117.6
O11ii—Ba2—N366.7 (3)C14—C15—H15117.6
O1—Ba2—N3128.4 (2)N6—C17—C18122.2 (12)
O9—Ba2—N390.1 (3)N6—C17—H17118.9
O13i—Ba2—N369.2 (3)C18—C17—H17118.9
O12ii—Ba2—N3102.4 (3)N5—C18—C17122.4 (13)
O14ii—Ba2—N3138.6 (3)N5—C18—H18118.8
O10i—Ba2—N3100.5 (3)C17—C18—H18118.8
O3—Ba2—Ba140.23 (16)O8—C19—O7126.1 (12)
O15i—Ba2—Ba1112.16 (17)O8—C19—C20116.8 (11)
O11ii—Ba2—Ba1109.98 (17)O7—C19—C20116.9 (11)
O1—Ba2—Ba138.65 (17)N7—C20—C21119.9 (12)
O9—Ba2—Ba139.87 (15)N7—C20—C19119.6 (11)
O13i—Ba2—Ba1127.78 (16)C21—C20—C19120.5 (11)
O12ii—Ba2—Ba1154.19 (16)N8—C21—C20123.6 (13)
O14ii—Ba2—Ba196.38 (17)N8—C21—H21118.2
O10i—Ba2—Ba179.64 (15)C20—C21—H21118.2
N3—Ba2—Ba192.17 (18)N8—C23—C24122.9 (14)
O3—Ba2—Ba1ii134.1 (2)N8—C23—H23118.6
O15i—Ba2—Ba1ii91.90 (17)C24—C23—H23118.6
O11ii—Ba2—Ba1ii36.55 (16)N7—C24—C23122.6 (14)
O1—Ba2—Ba1ii112.37 (18)N7—C24—H24118.7
O9—Ba2—Ba1ii78.29 (15)C23—C24—H24118.7
O1—Ba1—Ba2—O3139.0 (4)O11ii—Ba2—O1—Ba167.8 (4)
O11—Ba1—Ba2—O311.7 (4)O9—Ba2—O1—Ba142.4 (3)
O9—Ba1—Ba2—O3110.2 (4)O13i—Ba2—O1—Ba1111.8 (3)
O15—Ba1—Ba2—O3132.5 (4)O12ii—Ba2—O1—Ba1147.6 (2)
O14—Ba1—Ba2—O396.6 (4)O14ii—Ba2—O1—Ba1118.8 (3)
O10—Ba1—Ba2—O370.1 (5)O10i—Ba2—O1—Ba1106.6 (3)
O13—Ba1—Ba2—O359.2 (3)N3—Ba2—O1—Ba123.8 (5)
O12—Ba1—Ba2—O360.6 (4)Ba1ii—Ba2—O1—Ba1105.1 (2)
N1—Ba1—Ba2—O3162.4 (4)O15i—Ba2—O3—C7123.5 (11)
Ba2iv—Ba1—Ba2—O352.2 (3)O11ii—Ba2—O3—C757.0 (12)
O1—Ba1—Ba2—O15i10.9 (3)O1—Ba2—O3—C7173.3 (12)
O11—Ba1—Ba2—O15i116.4 (2)O9—Ba2—O3—C7119.2 (12)
O9—Ba1—Ba2—O15i121.7 (3)O13i—Ba2—O3—C751.2 (11)
O15—Ba1—Ba2—O15i99.5 (3)O12ii—Ba2—O3—C719.2 (15)
O3—Ba1—Ba2—O15i128.1 (4)O14ii—Ba2—O3—C7136.0 (11)
O14—Ba1—Ba2—O15i31.5 (3)O10i—Ba2—O3—C7106.1 (11)
O10—Ba1—Ba2—O15i161.8 (4)N3—Ba2—O3—C79.1 (11)
O13—Ba1—Ba2—O15i172.8 (2)Ba1—Ba2—O3—C7161.3 (13)
O12—Ba1—Ba2—O15i67.5 (2)Ba1ii—Ba2—O3—C781.7 (12)
N1—Ba1—Ba2—O15i34.3 (3)O15i—Ba2—O3—Ba175.2 (4)
Ba2iv—Ba1—Ba2—O15i75.88 (18)O11ii—Ba2—O3—Ba1104.3 (3)
O1—Ba1—Ba2—O11ii132.5 (4)O1—Ba2—O3—Ba125.4 (3)
O11—Ba1—Ba2—O11ii100.2 (3)O9—Ba2—O3—Ba142.1 (3)
O9—Ba1—Ba2—O11ii21.7 (3)O13i—Ba2—O3—Ba1147.5 (3)
O15—Ba1—Ba2—O11ii43.9 (2)O12ii—Ba2—O3—Ba1142.2 (5)
O3—Ba1—Ba2—O11ii88.5 (4)O14ii—Ba2—O3—Ba125.3 (5)
O14—Ba1—Ba2—O11ii174.9 (3)O10i—Ba2—O3—Ba192.6 (3)
O10—Ba1—Ba2—O11ii18.4 (4)N3—Ba2—O3—Ba1152.2 (4)
O13—Ba1—Ba2—O11ii29.4 (2)Ba1ii—Ba2—O3—Ba179.6 (3)
O12—Ba1—Ba2—O11ii149.1 (2)O1—Ba1—O3—C7171.1 (11)
N1—Ba1—Ba2—O11ii109.1 (3)O11—Ba1—O3—C728.6 (10)
Ba2iv—Ba1—Ba2—O11ii140.71 (17)O9—Ba1—O3—C7119.5 (11)
O11—Ba1—Ba2—O1127.3 (4)O15—Ba1—O3—C794.2 (11)
O9—Ba1—Ba2—O1110.8 (4)O14—Ba1—O3—C787.2 (11)
O15—Ba1—Ba2—O188.6 (3)O10—Ba1—O3—C714.0 (11)
O3—Ba1—Ba2—O1139.0 (4)O13—Ba1—O3—C743.8 (10)
O14—Ba1—Ba2—O142.4 (4)O12—Ba1—O3—C790.6 (10)
O10—Ba1—Ba2—O1150.9 (5)N1—Ba1—O3—C7174.5 (10)
O13—Ba1—Ba2—O1161.9 (3)Ba2—Ba1—O3—C7162.6 (12)
O12—Ba1—Ba2—O178.4 (4)Ba2iv—Ba1—O3—C762.3 (10)
N1—Ba1—Ba2—O123.4 (4)O1—Ba1—O3—Ba226.3 (3)
Ba2iv—Ba1—Ba2—O186.8 (3)O11—Ba1—O3—Ba2168.8 (3)
O1—Ba1—Ba2—O9110.8 (4)O9—Ba1—O3—Ba243.1 (3)
O11—Ba1—Ba2—O9121.9 (3)O15—Ba1—O3—Ba268.4 (4)
O15—Ba1—Ba2—O922.3 (3)O14—Ba1—O3—Ba2110.2 (3)
O3—Ba1—Ba2—O9110.2 (4)O10—Ba1—O3—Ba2148.6 (2)
O14—Ba1—Ba2—O9153.2 (3)O13—Ba1—O3—Ba2118.8 (3)
O10—Ba1—Ba2—O940.1 (4)O12—Ba1—O3—Ba2106.7 (3)
O13—Ba1—Ba2—O951.0 (3)N1—Ba1—O3—Ba222.9 (5)
O12—Ba1—Ba2—O9170.8 (3)Ba2iv—Ba1—O3—Ba2135.1 (2)
N1—Ba1—Ba2—O987.4 (3)O1—Ba1—O9—Ba241.9 (2)
Ba2iv—Ba1—Ba2—O9162.4 (3)O11—Ba1—O9—Ba280.6 (3)
O1—Ba1—Ba2—O13i96.4 (4)O15—Ba1—O9—Ba2158.3 (3)
O11—Ba1—Ba2—O13i30.9 (3)O3—Ba1—O9—Ba241.0 (2)
O9—Ba1—Ba2—O13i152.8 (3)O14—Ba1—O9—Ba265.4 (6)
O15—Ba1—Ba2—O13i175.1 (3)O10—Ba1—O9—Ba2161.4 (2)
O3—Ba1—Ba2—O13i42.6 (4)O13—Ba1—O9—Ba2125.4 (3)
O14—Ba1—Ba2—O13i54.0 (3)O12—Ba1—O9—Ba210.3 (4)
O10—Ba1—Ba2—O13i112.8 (4)N1—Ba1—O9—Ba293.6 (3)
O13—Ba1—Ba2—O13i101.8 (3)Ba2iv—Ba1—O9—Ba236.9 (5)
O12—Ba1—Ba2—O13i18.0 (3)O3—Ba2—O9—Ba142.5 (2)
N1—Ba1—Ba2—O13i119.8 (3)O15i—Ba2—O9—Ba180.5 (3)
Ba2iv—Ba1—Ba2—O13i9.6 (2)O11ii—Ba2—O9—Ba1158.7 (3)
O1—Ba1—Ba2—O12ii73.5 (5)O1—Ba2—O9—Ba141.0 (2)
O11—Ba1—Ba2—O12ii159.2 (4)O13i—Ba2—O9—Ba167.9 (6)
O9—Ba1—Ba2—O12ii37.3 (5)O12ii—Ba2—O9—Ba1162.6 (2)
O15—Ba1—Ba2—O12ii15.0 (4)O14ii—Ba2—O9—Ba1124.8 (3)
O3—Ba1—Ba2—O12ii147.5 (5)O10i—Ba2—O9—Ba18.9 (3)
O14—Ba1—Ba2—O12ii115.9 (4)N3—Ba2—O9—Ba193.2 (3)
O10—Ba1—Ba2—O12ii77.3 (5)Ba1ii—Ba2—O9—Ba1163.9 (2)
O13—Ba1—Ba2—O12ii88.3 (4)O1—Ba1—O10—Ba2iii86.2 (7)
O12—Ba1—Ba2—O12ii151.9 (6)O11—Ba1—O10—Ba2iii125.2 (3)
N1—Ba1—Ba2—O12ii50.2 (4)O9—Ba1—O10—Ba2iii4.2 (3)
Ba2iv—Ba1—Ba2—O12ii160.3 (4)O15—Ba1—O10—Ba2iii41.9 (2)
O1—Ba1—Ba2—O14ii59.0 (3)O3—Ba1—O10—Ba2iii79.9 (3)
O11—Ba1—Ba2—O14ii173.7 (2)O14—Ba1—O10—Ba2iii158.5 (3)
O9—Ba1—Ba2—O14ii51.8 (3)O13—Ba1—O10—Ba2iii45.2 (2)
O15—Ba1—Ba2—O14ii29.5 (2)O12—Ba1—O10—Ba2iii155.7 (2)
O3—Ba1—Ba2—O14ii162.0 (4)N1—Ba1—O10—Ba2iii93.2 (3)
O14—Ba1—Ba2—O14ii101.4 (3)Ba2—Ba1—O10—Ba2iii32.3 (5)
O10—Ba1—Ba2—O14ii91.9 (4)Ba2iv—Ba1—O10—Ba2iii161.9 (2)
O13—Ba1—Ba2—O14ii102.8 (2)O1—Ba1—O11—Ba2iv63.1 (4)
O12—Ba1—Ba2—O14ii137.4 (2)O9—Ba1—O11—Ba2iv148.9 (2)
N1—Ba1—Ba2—O14ii35.6 (3)O15—Ba1—O11—Ba2iv116.3 (3)
Ba2iv—Ba1—Ba2—O14ii145.83 (17)O3—Ba1—O11—Ba2iv112.9 (3)
O1—Ba1—Ba2—O10i61.3 (3)O14—Ba1—O11—Ba2iv17.6 (2)
O11—Ba1—Ba2—O10i66.0 (2)O10—Ba1—O11—Ba2iv102.8 (3)
O9—Ba1—Ba2—O10i172.1 (3)O13—Ba1—O11—Ba2iv165.8 (3)
O15—Ba1—Ba2—O10i149.8 (2)O12—Ba1—O11—Ba2iv45.1 (3)
O3—Ba1—Ba2—O10i77.7 (3)N1—Ba1—O11—Ba2iv21.6 (6)
O14—Ba1—Ba2—O10i18.9 (2)Ba2—Ba1—O11—Ba2iv105.4 (2)
O10—Ba1—Ba2—O10i147.8 (5)O1—Ba1—O12—Ba2iv151.1 (3)
O13—Ba1—Ba2—O10i136.9 (2)O11—Ba1—O12—Ba2iv43.1 (2)
O12—Ba1—Ba2—O10i17.1 (2)O9—Ba1—O12—Ba2iv161.2 (2)
N1—Ba1—Ba2—O10i84.7 (3)O15—Ba1—O12—Ba2iv62.6 (9)
Ba2iv—Ba1—Ba2—O10i25.53 (16)O3—Ba1—O12—Ba2iv130.6 (3)
O1—Ba1—Ba2—N3161.6 (4)O14—Ba1—O12—Ba2iv45.9 (2)
O11—Ba1—Ba2—N334.3 (3)O10—Ba1—O12—Ba2iv9.8 (4)
O9—Ba1—Ba2—N387.6 (3)O13—Ba1—O12—Ba2iv77.0 (3)
O15—Ba1—Ba2—N3109.9 (3)N1—Ba1—O12—Ba2iv101.8 (3)
O3—Ba1—Ba2—N322.6 (4)Ba2—Ba1—O12—Ba2iv167.9 (2)
O14—Ba1—Ba2—N3119.2 (3)O1—Ba1—O13—Ba2iii111.2 (3)
O10—Ba1—Ba2—N347.5 (4)O11—Ba1—O13—Ba2iii121.5 (3)
O13—Ba1—Ba2—N336.6 (3)O9—Ba1—O13—Ba2iii95.3 (3)
O12—Ba1—Ba2—N383.2 (3)O15—Ba1—O13—Ba2iii17.4 (2)
N1—Ba1—Ba2—N3175.0 (3)O3—Ba1—O13—Ba2iii160.6 (3)
Ba2iv—Ba1—Ba2—N374.8 (2)O14—Ba1—O13—Ba2iii78.9 (3)
O1—Ba1—Ba2—Ba1ii93.2 (3)O10—Ba1—O13—Ba2iii47.0 (2)
O11—Ba1—Ba2—Ba1ii139.50 (17)O12—Ba1—O13—Ba2iii151.9 (2)
O9—Ba1—Ba2—Ba1ii17.6 (3)N1—Ba1—O13—Ba2iii26.4 (5)
O15—Ba1—Ba2—Ba1ii4.63 (17)Ba2—Ba1—O13—Ba2iii127.36 (19)
O3—Ba1—Ba2—Ba1ii127.8 (3)Ba2iv—Ba1—O13—Ba2iii112.63 (19)
O14—Ba1—Ba2—Ba1ii135.59 (19)O1—Ba1—O14—Ba2iv114.2 (3)
O10—Ba1—Ba2—Ba1ii57.7 (4)O11—Ba1—O14—Ba2iv16.9 (2)
O13—Ba1—Ba2—Ba1ii68.66 (16)O9—Ba1—O14—Ba2iv135.3 (5)
O12—Ba1—Ba2—Ba1ii171.60 (17)O15—Ba1—O14—Ba2iv138.9 (2)
N1—Ba1—Ba2—Ba1ii69.8 (2)O3—Ba1—O14—Ba2iv42.1 (4)
Ba2iv—Ba1—Ba2—Ba1ii180.0O10—Ba1—O14—Ba2iv85.7 (3)
O1—Ba1—N1—C6175.3 (12)O13—Ba1—O14—Ba2iv58.5 (4)
O11—Ba1—N1—C670.4 (12)O12—Ba1—O14—Ba2iv45.8 (2)
O9—Ba1—N1—C6117.2 (11)N1—Ba1—O14—Ba2iv165.7 (4)
O15—Ba1—N1—C645.6 (11)Ba2—Ba1—O14—Ba2iv88.4 (2)
O3—Ba1—N1—C6171.4 (10)O1—Ba1—O15—Ba2iii149.8 (3)
O14—Ba1—N1—C674.5 (11)O11—Ba1—O15—Ba2iii30.7 (4)
O10—Ba1—N1—C61.7 (12)O9—Ba1—O15—Ba2iii93.2 (3)
O13—Ba1—N1—C655.0 (13)O3—Ba1—O15—Ba2iii69.9 (4)
O12—Ba1—N1—C6123.5 (11)O14—Ba1—O15—Ba2iii111.3 (3)
Ba2—Ba1—N1—C6157.4 (11)O10—Ba1—O15—Ba2iii45.1 (2)
Ba2iv—Ba1—N1—C683.8 (11)O13—Ba1—O15—Ba2iii17.9 (2)
O1—Ba1—N1—C21.8 (8)O12—Ba1—O15—Ba2iii126.1 (7)
O11—Ba1—N1—C2112.5 (9)N1—Ba1—O15—Ba2iii168.7 (4)
O9—Ba1—N1—C259.9 (9)Ba2—Ba1—O15—Ba2iii108.1 (2)
O15—Ba1—N1—C2131.5 (9)Ba2iv—Ba1—O15—Ba2iii77.5 (3)
O3—Ba1—N1—C25.7 (10)Ba1—O1—C1—O2168.9 (9)
O14—Ba1—N1—C2108.4 (9)Ba2—O1—C1—O236.7 (17)
O10—Ba1—N1—C2178.8 (9)Ba1—O1—C1—C211.6 (16)
O13—Ba1—N1—C2122.1 (8)Ba2—O1—C1—C2142.7 (9)
O12—Ba1—N1—C259.4 (9)C6—N1—C2—C34 (2)
Ba2—Ba1—N1—C219.7 (9)Ba1—N1—C2—C3178.6 (11)
Ba2iv—Ba1—N1—C299.1 (9)C6—N1—C2—C1179.5 (12)
O3—Ba2—N3—C82.1 (8)Ba1—N1—C2—C12.1 (14)
O15i—Ba2—N3—C8112.3 (9)O2—C1—C2—N1172.2 (12)
O11ii—Ba2—N3—C8130.5 (10)O1—C1—C2—N18.3 (17)
O1—Ba2—N3—C85.0 (11)O2—C1—C2—C34.3 (19)
O9—Ba2—N3—C859.5 (9)O1—C1—C2—C3175.2 (13)
O13i—Ba2—N3—C8110.3 (9)C5—N2—C3—C23 (2)
O12ii—Ba2—N3—C8178.2 (9)N1—C2—C3—N24 (2)
O14ii—Ba2—N3—C8121.8 (9)C1—C2—C3—N2179.2 (13)
O10i—Ba2—N3—C860.2 (9)C3—N2—C5—C62 (2)
Ba1—Ba2—N3—C819.6 (9)C2—N1—C6—C53 (2)
Ba1ii—Ba2—N3—C8137.5 (9)Ba1—N1—C6—C5180.0 (11)
O3—Ba2—N3—C12175.7 (12)N2—C5—C6—N12 (3)
O15i—Ba2—N3—C1269.9 (12)Ba2—O3—C7—O4168.8 (10)
O11ii—Ba2—N3—C1247.3 (11)Ba1—O3—C7—O434 (2)
O1—Ba2—N3—C12172.8 (10)Ba2—O3—C7—C814.4 (18)
O9—Ba2—N3—C12118.4 (11)Ba1—O3—C7—C8143.0 (9)
O13i—Ba2—N3—C1271.9 (11)C12—N3—C8—C93.1 (19)
O12ii—Ba2—N3—C120.3 (11)Ba2—N3—C8—C9178.9 (10)
O14ii—Ba2—N3—C1256.0 (12)C12—N3—C8—C7179.2 (12)
O10i—Ba2—N3—C12121.9 (11)Ba2—N3—C8—C72.7 (15)
Ba1—Ba2—N3—C12158.2 (11)O3—C7—C8—N310.2 (19)
Ba1ii—Ba2—N3—C1240.4 (11)O4—C7—C8—N3172.7 (12)
O11—Ba1—O1—C1125.4 (10)O3—C7—C8—C9173.7 (13)
O9—Ba1—O1—C1116.7 (11)O4—C7—C8—C93 (2)
O15—Ba1—O1—C154.1 (10)C11—N4—C9—C81 (2)
O3—Ba1—O1—C1175.8 (11)N3—C8—C9—N43 (2)
O14—Ba1—O1—C154.1 (10)C7—C8—C9—N4179.0 (14)
O10—Ba1—O1—C115.7 (15)C9—N4—C11—C121 (2)
O13—Ba1—O1—C1133.5 (9)C8—N3—C12—C111 (2)
O12—Ba1—O1—C1109.5 (10)Ba2—N3—C12—C11178.9 (11)
N1—Ba1—O1—C17.4 (9)N4—C11—C12—N31 (3)
Ba2—Ba1—O1—C1158.9 (12)C18—N5—C14—C151.2 (19)
Ba2iv—Ba1—O1—C191.0 (10)C18—N5—C14—C13177.9 (13)
O11—Ba1—O1—Ba275.7 (4)O5—C13—C14—N50.9 (18)
O9—Ba1—O1—Ba242.2 (3)O6—C13—C14—N5178.8 (12)
O15—Ba1—O1—Ba2104.9 (3)O5—C13—C14—C15178.1 (12)
O3—Ba1—O1—Ba225.3 (3)O6—C13—C14—C150.2 (19)
O14—Ba1—O1—Ba2147.0 (3)C17—N6—C15—C141 (2)
O10—Ba1—O1—Ba2143.3 (6)N5—C14—C15—N60 (2)
O13—Ba1—O1—Ba225.4 (5)C13—C14—C15—N6178.9 (14)
O12—Ba1—O1—Ba291.5 (3)C15—N6—C17—C182 (2)
N1—Ba1—O1—Ba2151.5 (4)C14—N5—C18—C171 (2)
Ba2iv—Ba1—O1—Ba2110.1 (2)N6—C17—C18—N51 (3)
O3—Ba2—O1—C1173.6 (10)C24—N7—C20—C212 (2)
O15i—Ba2—O1—C130.4 (9)C24—N7—C20—C19178.0 (13)
O11ii—Ba2—O1—C192.3 (10)O8—C19—C20—N7173.2 (13)
O9—Ba2—O1—C1117.8 (10)O7—C19—C20—N72.0 (19)
O13i—Ba2—O1—C188.1 (10)O8—C19—C20—C217.2 (19)
O12ii—Ba2—O1—C112.5 (11)O7—C19—C20—C21177.6 (13)
O14ii—Ba2—O1—C141.3 (9)C23—N8—C21—C201 (2)
O10i—Ba2—O1—C193.3 (10)N7—C20—C21—N81 (2)
N3—Ba2—O1—C1176.1 (9)C19—C20—C21—N8179.1 (14)
Ba1—Ba2—O1—C1160.1 (11)C21—N8—C23—C243 (2)
Ba1ii—Ba2—O1—C155.0 (10)C20—N7—C24—C231 (2)
O3—Ba2—O1—Ba126.3 (3)N8—C23—C24—N72 (3)
O15i—Ba2—O1—Ba1169.5 (3)
Symmetry codes: (i) x, y, z1; (ii) x+1, y, z; (iii) x, y, z+1; (iv) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10A···O70.852.233.000 (13)152
O10—H10B···O50.851.922.769 (11)177
O11—H11A···O40.851.882.669 (12)153
O11—H11B···O50.852.042.861 (12)163
O11—H11B···N50.852.623.191 (14)126
O13—H13A···N50.852.142.983 (14)175
O14—H14A···O80.851.872.685 (12)160
O9—H9A···O7ii0.851.882.677 (12)155
O9—H9B···O5ii0.851.892.689 (12)156
O13—H13B···O6ii0.851.932.729 (12)157
O15—H15A···O7ii0.852.042.860 (12)161
O15—H15A···N7ii0.852.623.208 (14)127
O12—H12A···O7i0.851.962.811 (12)179
O12—H12B···O5i0.852.263.018 (12)149
O14—H14B···N7i0.852.183.028 (13)174
O15—H15B···O2iii0.851.902.676 (11)152
Symmetry codes: (i) x, y, z1; (ii) x+1, y, z; (iii) x, y, z+1.

Experimental details

Crystal data
Chemical formula[Ba2(C5H3N2O2)2(H2O)7](C5H3N2O2)2
Mr893.17
Crystal system, space groupMonoclinic, P21
Temperature (K)298
a, b, c (Å)7.5652 (10), 29.263 (3), 7.6067 (10)
β (°) 118.741 (2)
V3)1476.5 (3)
Z2
Radiation typeMo Kα
µ (mm1)2.74
Crystal size (mm)0.49 × 0.34 × 0.16
Data collection
DiffractometerBruker SMART APEX CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2002)
Tmin, Tmax0.348, 0.669
No. of measured, independent and
observed [I > 2σ(I)] reflections
7342, 4734, 4502
Rint0.036
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.046, 0.121, 1.02
No. of reflections4734
No. of parameters406
No. of restraints1
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.062P)2 + 10.4333P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.84, 2.62
Absolute structureFlack (1983), 2096 Friedel pairs
Absolute structure parameter0.04 (4)

Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10A···O70.852.233.000 (13)152
O10—H10B···O50.851.922.769 (11)177
O11—H11A···O40.851.882.669 (12)153
O11—H11B···O50.852.042.861 (12)163
O11—H11B···N50.852.623.191 (14)126
O13—H13A···N50.852.142.983 (14)175
O14—H14A···O80.851.872.685 (12)160
O9—H9A···O7i0.851.882.677 (12)155
O9—H9B···O5i0.851.892.689 (12)156
O13—H13B···O6i0.851.932.729 (12)157
O15—H15A···O7i0.852.042.860 (12)161
O15—H15A···N7i0.852.623.208 (14)127
O12—H12A···O7ii0.851.962.811 (12)179
O12—H12B···O5ii0.852.263.018 (12)149
O14—H14B···N7ii0.852.183.028 (13)174
O15—H15B···O2iii0.851.902.676 (11)152
Symmetry codes: (i) x+1, y, z; (ii) x, y, z1; (iii) x, y, z+1.
 

Acknowledgements

This work was supported by the Scientific Research Foundation of Northwest A&F University (grant No. Z111020828).

References

First citationBruker (2002). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationFlack, H. D. (1983). Acta Cryst. A39, 876–881.  CrossRef CAS Web of Science IUCr Journals Google Scholar
First citationHuang, D., Zhang, X., Chen, C., Chen, F., Liu, Q., Liao, D., Li, L. & Sun, L. (2003). Inorg. Chim. Acta, 353, 284–291.  Web of Science CSD CrossRef CAS Google Scholar
First citationPtasiewicz-Bak, H., Ostrowski, A. & Leciejewicz, J. (1998). Pol. J. Chem. 72, 2014–2023.  CAS Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationYin, H. D., Li, G., Gao, Z. J. & Xu, H. L. (2006). J. Organomet. Chem. 691, 1235–1241.  Web of Science CSD CrossRef CAS Google Scholar

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Volume 67| Part 2| February 2011| Pages m283-m284
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