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A nickel(II) coordination polymer, catena-poly[[aqua­tri­pyri­dinenickel(II)]-μ-isophthalato], [Ni(C8H4O4)(C5H5N)3(H2O)]n, obtained by reaction of m-bda, pyridine and Ni(NO3)2·6H2O under hydro­thermal conditions, where m-bda is isophthalic acid, was characterized by single-crystal X-ray diffraction. The NiII atom is six-coordinate and lies at the centre of a distorted octa­hedron, coordinated by two carboxylate O atoms from two m-bda ligands, three N atoms from three pyridine mol­ecules and one water mol­ecule. The carboxylate groups of m-bda link the NiII atoms, forming an extended one-dimensional zigzag chain. The chains are then knitted together, forming a two-dimensional supramolecular arrangement, via C—H...O hydrogen bonds between the H atoms of pyridine rings and the coordinated carboxylate O atoms of m-bda.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680600153X/wk6070sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680600153X/wk6070Isup2.hkl
Contains datablock I

CCDC reference: 298561

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.038
  • wR factor = 0.071
  • Data-to-parameter ratio = 18.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.87 Ratio
Author Response: There are two H atoms bond to the water O5W atom. Both of the H atoms have hydrogen-bond interaction, which results in the large Ueq Ratio (Ueq(H5B)/Ueq(H5A))
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .      78.00 A   3  

0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 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 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97.

catena-poly[[aquatripyridinenickel(II)]-µ-isophthalato] top
Crystal data top
[Ni(C8H4O4)(C5H5N)3(H2O)]F(000) = 992
Mr = 478.14Dx = 1.385 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 9.0723 (5) ÅCell parameters from 13853 reflections
b = 15.1897 (8) Åθ = 1.8–28.2°
c = 16.6524 (9) ŵ = 0.88 mm1
β = 91.886 (1)°T = 293 K
V = 2293.5 (2) Å3Block, blue
Z = 40.35 × 0.29 × 0.23 mm
Data collection top
Rigaku R-AXIS RAPID
diffractometer
5392 independent reflections
Radiation source: fine-focus sealed tube2787 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
Detector resolution: 10.0 pixels mm-1θmax = 28.3°, θmin = 1.8°
ω scansh = 1211
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1920
Tmin = 0.751, Tmax = 0.814l = 2215
14005 measured reflections
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)] = 0.038Hydrogen site location: geom and difmap
wR(F2) = 0.071H atoms treated by a mixture of independent and constrained refinement
S = 1.01 w = 1/[σ2(Fo2) + (0.0201P)2]
where P = (Fo2 + 2Fc2)/3
5392 reflections(Δ/σ)max = 0.001
297 parametersΔρmax = 0.29 e Å3
0 restraintsΔρmin = 0.39 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
C10.1103 (3)0.28392 (15)0.07613 (14)0.0542 (7)
H10.02190.29110.05010.065*
C20.2400 (3)0.29249 (16)0.03144 (15)0.0607 (7)
H20.23860.30570.02310.073*
C30.3715 (3)0.28119 (14)0.06883 (16)0.0604 (7)
H30.46090.28570.04010.072*
C40.3675 (3)0.26319 (15)0.14910 (16)0.0601 (7)
H40.45450.25550.17620.072*
C50.2340 (3)0.25659 (14)0.18927 (14)0.0567 (6)
H50.23330.24490.24410.068*
C60.3616 (3)0.29492 (16)0.32772 (14)0.0539 (7)
H60.31520.34950.32660.065*
C70.4910 (3)0.28624 (18)0.37249 (14)0.0606 (7)
H70.53020.33380.40110.073*
C80.5613 (3)0.20643 (19)0.37424 (15)0.0638 (7)
H80.64840.19850.40440.077*
C90.5001 (3)0.13842 (17)0.33039 (14)0.0609 (7)
H90.54600.08370.32970.073*
C100.3699 (3)0.15199 (16)0.28735 (13)0.0535 (7)
H100.32940.10520.25810.064*
C110.0073 (3)0.13249 (15)0.35274 (14)0.0530 (6)
H110.03160.17850.38360.064*
C120.0809 (3)0.06672 (17)0.39078 (16)0.0760 (9)
H120.09320.06840.44600.091*
C130.1363 (3)0.00209 (18)0.3452 (2)0.0880 (10)
H130.18770.04760.36910.106*
C140.1149 (3)0.00271 (16)0.26429 (18)0.0768 (9)
H140.14960.04900.23240.092*
C150.0411 (3)0.06655 (15)0.23119 (15)0.0578 (7)
H150.02720.06610.17610.069*
C160.2371 (2)0.19310 (15)0.06644 (12)0.0401 (5)
C170.2821 (2)0.11976 (14)0.01114 (12)0.0377 (5)
C180.2480 (3)0.03284 (15)0.02536 (14)0.0568 (7)
H180.19590.01800.07060.068*
C190.2902 (3)0.03237 (15)0.02684 (15)0.0685 (8)
H190.26690.09080.01650.082*
C200.3673 (3)0.01087 (15)0.09455 (14)0.0575 (7)
H200.39590.05500.12940.069*
C210.4019 (2)0.07581 (13)0.11053 (12)0.0397 (6)
C220.3590 (2)0.13961 (14)0.05730 (11)0.0382 (5)
H220.38250.19810.06760.046*
C230.4862 (2)0.10101 (15)0.18384 (13)0.0445 (6)
H5A0.115 (3)0.3905 (15)0.1643 (15)0.063 (10)*
H5B0.211 (4)0.350 (2)0.123 (2)0.178 (18)*
N10.1041 (2)0.26605 (11)0.15418 (11)0.0485 (5)
N20.01153 (19)0.13409 (11)0.27380 (11)0.0433 (5)
N30.2992 (2)0.22878 (12)0.28557 (11)0.0463 (5)
Ni10.09974 (3)0.247460 (19)0.219975 (15)0.04269 (10)
O10.17270 (16)0.16992 (9)0.12911 (8)0.0477 (4)
O20.26464 (17)0.27053 (9)0.04662 (9)0.0534 (4)
O30.52068 (16)0.18125 (9)0.18790 (8)0.0493 (4)
O40.5149 (2)0.04519 (10)0.23416 (11)0.0884 (7)
O5W0.1940 (3)0.36099 (13)0.17545 (12)0.0671 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0531 (17)0.0724 (17)0.0376 (15)0.0047 (13)0.0090 (12)0.0022 (13)
C20.0583 (19)0.0849 (18)0.0388 (15)0.0125 (15)0.0015 (14)0.0018 (14)
C30.0508 (18)0.0684 (17)0.0613 (18)0.0000 (13)0.0073 (14)0.0084 (14)
C40.0490 (17)0.0680 (18)0.0641 (18)0.0028 (14)0.0121 (13)0.0060 (15)
C50.0591 (17)0.0661 (16)0.0456 (14)0.0027 (15)0.0137 (12)0.0133 (14)
C60.0579 (18)0.0552 (15)0.0491 (16)0.0088 (13)0.0103 (13)0.0090 (13)
C70.0551 (19)0.0796 (19)0.0470 (17)0.0148 (16)0.0014 (14)0.0147 (14)
C80.0512 (18)0.091 (2)0.0489 (17)0.0000 (17)0.0015 (13)0.0049 (16)
C90.0528 (18)0.0722 (18)0.0578 (18)0.0020 (15)0.0027 (14)0.0082 (15)
C100.0498 (18)0.0637 (17)0.0473 (16)0.0088 (14)0.0045 (13)0.0104 (14)
C110.0658 (18)0.0524 (15)0.0410 (15)0.0009 (13)0.0035 (12)0.0075 (13)
C120.111 (3)0.0617 (17)0.0571 (19)0.0019 (17)0.0236 (18)0.0186 (16)
C130.110 (3)0.0586 (19)0.097 (3)0.0126 (18)0.028 (2)0.0238 (19)
C140.093 (2)0.0579 (18)0.080 (2)0.0242 (16)0.0025 (18)0.0017 (16)
C150.0621 (19)0.0596 (16)0.0519 (17)0.0099 (14)0.0060 (13)0.0039 (14)
C160.0305 (13)0.0582 (16)0.0316 (13)0.0014 (11)0.0006 (10)0.0026 (12)
C170.0333 (13)0.0465 (13)0.0333 (13)0.0017 (11)0.0035 (10)0.0004 (11)
C180.0687 (19)0.0576 (15)0.0454 (15)0.0088 (13)0.0224 (13)0.0021 (13)
C190.098 (2)0.0445 (14)0.0645 (18)0.0176 (14)0.0303 (16)0.0039 (14)
C200.0753 (19)0.0474 (14)0.0511 (16)0.0067 (13)0.0208 (13)0.0095 (13)
C210.0406 (15)0.0426 (13)0.0364 (13)0.0032 (11)0.0067 (11)0.0067 (11)
C220.0355 (14)0.0444 (13)0.0349 (12)0.0001 (10)0.0027 (10)0.0011 (11)
C230.0479 (16)0.0469 (14)0.0392 (15)0.0026 (12)0.0101 (12)0.0070 (13)
N10.0520 (13)0.0564 (13)0.0378 (11)0.0039 (10)0.0116 (9)0.0035 (10)
N20.0452 (13)0.0483 (12)0.0366 (12)0.0034 (9)0.0049 (9)0.0010 (10)
N30.0461 (12)0.0521 (13)0.0412 (12)0.0054 (10)0.0088 (9)0.0065 (10)
Ni10.04917 (18)0.04774 (17)0.03189 (15)0.00513 (16)0.01236 (12)0.00088 (16)
O10.0577 (11)0.0531 (9)0.0333 (9)0.0062 (8)0.0158 (8)0.0024 (8)
O20.0672 (12)0.0472 (10)0.0473 (10)0.0008 (8)0.0242 (8)0.0002 (8)
O30.0687 (12)0.0436 (9)0.0369 (9)0.0021 (8)0.0220 (8)0.0018 (8)
O40.1388 (19)0.0555 (11)0.0751 (14)0.0217 (11)0.0655 (13)0.0240 (10)
O5W0.0863 (17)0.0588 (12)0.0579 (13)0.0081 (12)0.0292 (12)0.0020 (11)
Geometric parameters (Å, º) top
C1—N11.327 (3)C14—C151.372 (3)
C1—C21.378 (3)C14—H140.9300
C1—H10.9300C15—N21.327 (2)
C2—C31.374 (3)C15—H150.9300
C2—H20.9300C16—O21.249 (2)
C3—C41.364 (3)C16—O11.263 (2)
C3—H30.9300C16—C171.510 (3)
C4—C51.367 (3)C17—C181.378 (3)
C4—H40.9300C17—C221.389 (2)
C5—N11.340 (3)C18—C191.380 (3)
C5—H50.9300C18—H180.9300
C6—N31.341 (3)C19—C201.385 (3)
C6—C71.376 (3)C19—H190.9300
C6—H60.9300C20—C211.381 (3)
C7—C81.370 (3)C20—H200.9300
C7—H70.9300C21—C221.378 (2)
C8—C91.372 (3)C21—C231.511 (3)
C8—H80.9300C22—H220.9300
C9—C101.377 (3)C23—O41.226 (2)
C9—H90.9300C23—O31.261 (2)
C10—N31.331 (3)N1—Ni12.1372 (19)
C10—H100.9300N2—Ni12.1110 (17)
C11—N21.331 (2)N3—Ni12.102 (2)
C11—C121.368 (3)Ni1—O3i2.0280 (13)
C11—H110.9300Ni1—O12.0446 (13)
C12—C131.377 (3)Ni1—O5W2.0727 (17)
C12—H120.9300O3—Ni1ii2.0280 (13)
C13—C141.367 (4)O5W—H5A0.86 (2)
C13—H130.9300O5W—H5B0.90 (4)
N1—C1—C2123.8 (2)C18—C17—C16122.34 (18)
N1—C1—H1118.1C22—C17—C16119.58 (19)
C2—C1—H1118.1C17—C18—C19120.7 (2)
C3—C2—C1118.8 (2)C17—C18—H18119.7
C3—C2—H2120.6C19—C18—H18119.7
C1—C2—H2120.6C18—C19—C20120.1 (2)
C4—C3—C2118.3 (2)C18—C19—H19120.0
C4—C3—H3120.9C20—C19—H19120.0
C2—C3—H3120.9C21—C20—C19120.4 (2)
C3—C4—C5119.3 (2)C21—C20—H20119.8
C3—C4—H4120.4C19—C20—H20119.8
C5—C4—H4120.4C22—C21—C20118.40 (19)
N1—C5—C4123.8 (2)C22—C21—C23120.17 (18)
N1—C5—H5118.1C20—C21—C23121.42 (19)
C4—C5—H5118.1C21—C22—C17122.35 (19)
N3—C6—C7123.4 (2)C21—C22—H22118.8
N3—C6—H6118.3C17—C22—H22118.8
C7—C6—H6118.3O4—C23—O3125.0 (2)
C8—C7—C6119.0 (2)O4—C23—C21120.1 (2)
C8—C7—H7120.5O3—C23—C21114.92 (19)
C6—C7—H7120.5C1—N1—C5116.1 (2)
C7—C8—C9118.4 (2)C1—N1—Ni1122.47 (15)
C7—C8—H8120.8C5—N1—Ni1121.39 (16)
C9—C8—H8120.8C15—N2—C11117.26 (19)
C8—C9—C10119.3 (2)C15—N2—Ni1122.57 (15)
C8—C9—H9120.3C11—N2—Ni1119.79 (16)
C10—C9—H9120.3C10—N3—C6116.7 (2)
N3—C10—C9123.2 (2)C10—N3—Ni1122.41 (16)
N3—C10—H10118.4C6—N3—Ni1120.86 (16)
C9—C10—H10118.4O3i—Ni1—O1176.88 (6)
N2—C11—C12123.4 (2)O3i—Ni1—O5W89.24 (7)
N2—C11—H11118.3O1—Ni1—O5W93.85 (7)
C12—C11—H11118.3O3i—Ni1—N389.93 (7)
C11—C12—C13118.3 (3)O1—Ni1—N390.73 (6)
C11—C12—H12120.9O5W—Ni1—N386.56 (8)
C13—C12—H12120.9O3i—Ni1—N288.05 (6)
C14—C13—C12119.2 (3)O1—Ni1—N288.90 (6)
C14—C13—H13120.4O5W—Ni1—N2175.67 (8)
C12—C13—H13120.4N3—Ni1—N290.06 (7)
C13—C14—C15118.5 (3)O3i—Ni1—N189.74 (6)
C13—C14—H14120.7O1—Ni1—N189.57 (6)
C15—C14—H14120.7O5W—Ni1—N193.84 (8)
N2—C15—C14123.3 (2)N3—Ni1—N1179.48 (7)
N2—C15—H15118.3N2—Ni1—N189.52 (7)
C14—C15—H15118.3C16—O1—Ni1128.38 (14)
O2—C16—O1125.7 (2)C23—O3—Ni1ii130.64 (14)
O2—C16—C17118.22 (18)Ni1—O5W—H5A99.1 (16)
O1—C16—C17116.12 (19)Ni1—O5W—H5B106 (2)
C18—C17—C22118.08 (19)H5A—O5W—H5B94 (3)
N1—C1—C2—C30.7 (4)C12—C11—N2—Ni1171.24 (19)
C1—C2—C3—C40.9 (3)C9—C10—N3—C60.7 (3)
C2—C3—C4—C50.3 (3)C9—C10—N3—Ni1179.56 (16)
C3—C4—C5—N10.6 (4)C7—C6—N3—C101.1 (3)
N3—C6—C7—C80.4 (4)C7—C6—N3—Ni1179.19 (17)
C6—C7—C8—C90.6 (3)C10—N3—Ni1—O3i138.67 (17)
C7—C8—C9—C101.0 (3)C6—N3—Ni1—O3i41.64 (16)
C8—C9—C10—N30.3 (4)C10—N3—Ni1—O138.28 (17)
N2—C11—C12—C131.1 (4)C6—N3—Ni1—O1141.42 (15)
C11—C12—C13—C140.6 (4)C10—N3—Ni1—O5W132.09 (18)
C12—C13—C14—C151.3 (5)C6—N3—Ni1—O5W47.60 (16)
C13—C14—C15—N20.4 (4)C10—N3—Ni1—N250.62 (17)
O2—C16—C17—C18175.8 (2)C6—N3—Ni1—N2129.68 (16)
O1—C16—C17—C183.6 (3)C15—N2—Ni1—O3i146.89 (17)
O2—C16—C17—C223.4 (3)C11—N2—Ni1—O3i25.89 (16)
O1—C16—C17—C22177.3 (2)C15—N2—Ni1—O132.45 (17)
C22—C17—C18—C190.4 (4)C11—N2—Ni1—O1154.77 (17)
C16—C17—C18—C19179.6 (2)C15—N2—Ni1—N3123.18 (17)
C17—C18—C19—C200.2 (4)C11—N2—Ni1—N364.04 (17)
C18—C19—C20—C210.3 (4)C15—N2—Ni1—N157.13 (17)
C19—C20—C21—C220.6 (4)C11—N2—Ni1—N1115.65 (17)
C19—C20—C21—C23179.9 (2)C1—N1—Ni1—O3i138.26 (17)
C20—C21—C22—C170.3 (3)C5—N1—Ni1—O3i44.56 (17)
C23—C21—C22—C17179.6 (2)C1—N1—Ni1—O144.79 (17)
C18—C17—C22—C210.2 (3)C5—N1—Ni1—O1132.39 (17)
C16—C17—C22—C21179.33 (19)C1—N1—Ni1—O5W49.04 (18)
C22—C21—C23—O4174.7 (2)C5—N1—Ni1—O5W133.78 (17)
C20—C21—C23—O46.0 (4)C1—N1—Ni1—N2133.69 (17)
C22—C21—C23—O34.7 (3)C5—N1—Ni1—N243.49 (17)
C20—C21—C23—O3174.6 (2)O2—C16—O1—Ni12.5 (3)
C2—C1—N1—C50.2 (3)C17—C16—O1—Ni1178.19 (13)
C2—C1—N1—Ni1177.10 (18)O5W—Ni1—O1—C166.73 (19)
C4—C5—N1—C10.9 (3)N3—Ni1—O1—C1693.34 (18)
C4—C5—N1—Ni1176.46 (18)N2—Ni1—O1—C16176.61 (18)
C14—C15—N2—C111.2 (3)N1—Ni1—O1—C1687.09 (18)
C14—C15—N2—Ni1171.8 (2)O4—C23—O3—Ni1ii11.4 (4)
C12—C11—N2—C151.9 (3)C21—C23—O3—Ni1ii167.96 (14)
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1/2, y+1/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5W—H5B···O20.94 (4)1.81 (4)2.647 (3)146 (4)
O5W—H5A···O4i0.87 (3)2.18 (3)2.664 (3)115 (2)
C3—H3···O2iii0.932.513.315 (4)145
C8—H8···O2iv0.932.603.378 (3)141
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (iii) x1, y, z; (iv) x+1/2, y+1/2, z+1/2.
 

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