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C29H31N5Ni2O15, monoclinic, P21 (no. 4), a = 10.823(2) Å, b = 10.750(2) Å, c = 13.582(3) Å, / = 94.64(3)°, V = 1575.1 Å, Z = 2, Rgt(F) = 0.052, wRref(F) = 0.113, T = 153 K. Source of material Reaction of 0.1 mmol pyridine-2,3,5,6-tetracarboxylic acid (PTA), 0.2 mmol Ni(NO3)2 · 6H2O and 0.2 mmol 2,2'-bipyridine dissolved in 10 mL aqueous methanol (1:1, v/v) yields a green solution. After filtering the solution, the filtrate is allowed to evaporate at room temperature whereupon green crystals of the title compound appeared after one month in the form of rectangular blocks in 65 % yield. Elemental analysis — found: C, 43.19 %; H, 3.89 %; N, 8.65 %; calculated for C29H31N5Ni2O15: C, 43.16 %; H, 3.87 %; N, 8.68 %. Discussion The crystal structure of the title complex can be described as a 1D coordination polymer of two types of hexacoordinated Ni(II) ions bonded ligands. To maintain charge balance, the ligand acid molecule remains fully deprotonated. Here, Ni2 ion is axially bonded to one carboxylate O atom from the PTA4− ligand and one O atom of one water molecule. The equatorial sites of Ni2 are occupied by two O atoms of two water molecules and two N atoms belonging to one 2,2'-bipyridine molecule. Both, the carboxylate groups and the ring N atom on one side of the PTA4− ligand bind Ni1 showing NO2 coordination leaving one O atom on each carboxylate free. Two N atoms of one 2,2'-bipyridine molecule and one O atom from another PTA4− ligand bind this Ni(II) ion to complete hexacoordination. Thus, Ni1 ions are bridged by PTA4− ligand to form the coordination polymeric chain along [010]. The bond distances and bond angles involving the metal ions are similar to those found in other octahedral Ni(II) complexes. Out of the water molecules the group of seven forms a (H2O)7 cluster. These clusters further assemble the 1D zigzag chains into an overall 3D MOF. A wide variation in the O-O nonbonding distances is found. These distances span the range 3.441 2.623 Å. The O−O−O angles also vary widely (range 125° 176°). In (H2O)7 cluster, O9 and O10 act as mono-donor, O15 acts as double-donors while the rest act as donors and acceptors of H bonding. So, not every O atom in the cluster shows four-coordination just like water molecules at the surface of the ice or liquid water. Z. Kristallogr. NCS 224 (2009) 469-470 / DOI 10.1524/ncrs.2009.0204 469 © by Oldenbourg Wissenschaftsverlag, München Crystal: green plate, size 0.02 × 0.02 × 0.04 mm Wavelength: Mo K1 radiation (0.71073 Å) ': 12.80 cm−1 Diffractometer, scan mode: Bruker SMART-1000, 3 2#max: 50.04° N(hkl)measured, N(hkl)unique: 9717, 5205 Criterion for Iobs, N(hkl)gt: Iobs > 2 "(Iobs), 4615 N(param)refined: 461 Programs: SHELXS-97 [1], SHELXL-97 [2], SHELXTL [3] Table 1. Data collection and handling. H(9B) 2a 0.4060 0.3463 0.4462 0.059 H(9A) 2a 0.3382 0.3279 0.5284 0.059 H(10B) 2a 0.2913 0.5896 0.6616 0.026 H(10A) 2a 0.2614 0.4655 0.6477 0.026 H(11B) 2a 0.5163 0.6399 0.4818 0.030 H(11A) 2a 0.5032 0.5977 0.5767 0.030 H(12A) 2a 0.6232 0.4900 0.6859 0.045 H(12B) 2a 0.6145 0.6042 0.7306 0.045 H(13A) 2a 0.3800 0.7446 0.2828 0.043 H(13B) 2a 0.3974 0.8282 0.2079 0.043 H(14A) 2a 0.5739 0.1876 0.2102 0.034 H(14B) 2a 0.6087 0.2732 0.2825 0.034 H(15A) 2a 0.6914 0.3428 0.0357 0.045 H(15B) 2a 0.7129 0.2988 0.1309 0.045 C(2) 2a 0.5949(5) 0.6224(6) 0.0365(4) 0.016(1) C(3) 2a 0.5149(5) 0.5211(5) 0.0359(4) 0.016(1) H(4) 2a 0.4180 0.4160 0.1270 0.020 C(5) 2a 0.5137(4) 0.5423(6) 0.2126(4) 0.015(1) C(7) 2a 0.6589(5) 0.7129(6) 0.2943(4) 0.016(1) H(10) 2a 0.7937 1.0933 0.1280 0.032 H(11) 2a 0.9578 1.2344 0.1479 0.036 H(12) 2a 1.1626 1.1580 0.1734 0.029 H(13) 2a 1.1963 0.9415 0.1616 0.034 H(16) 2a 1.2117 0.7423 0.1306 0.039 H(17) 2a 1.2103 0.5258 0.1090 0.046 Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso

zeitschrift für kristallographie. new crystal structures/zeitschrift für kristallographie. new crystal structures

Crystal structure of catena-triaqua-bis(2,2'-bipyridyl)-(pyridin- 2,3,5,6-tetracarboxylato-N,O,O')nickel(II) tetrahydrate, Ni 2 (H 2 O) 3 (C 10 H 8 N 2 ) 2 (C 9 HO 8 N) · 4H 2 O