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The two Ni atoms and the μ6-1,2,4,5-benzene­tetra­carboxyl­ate ligand in the crystal structure of catena-[μ6-1,2,4,5-benzene­tetra­carboxyl­ato-tetra­aqua-dinickel(II)] dihydrate, [Ni2(C10H2O8)(H2O)4]·2(H2O), occupy special positions at three independent inversion centers. One of the Ni atoms is chelated by two 1,2,4,5-benzene­tetra­carboxyl­ates [Ni—O 2.018 (3) and 2.021 (3) Å; O—Ni—O 91.7 (1)°]; the two remaining sites of the coordination octahedron of this atom are taken up by water mol­ecules. The second Ni atom is coordinated by four carbonyl O atoms belonging to four benzene­tetra­carboxyl­ate ligands [Ni—O 2.045 (3), 2.069 (3) Å]; its coordin­ation sphere also includes two water mol­ecules. Each tetraanionic benzene­tetra­carboxyl­ate ligand links together six Ni atoms, the linkages giving rise to a three-dimensional network motif. The structure is consolidated by hydrogen bonds involving coordinated as well as uncoordin­ated water mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803019196/ya6173sup1.cif
Contains datablocks I, ya6173

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803019196/ya6173Isup2.hkl
Contains datablock I

CCDC reference: 225653

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.005 Å
  • H-atom completeness 72%
  • R factor = 0.046
  • wR factor = 0.108
  • Data-to-parameter ratio = 16.9

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT430_ALERT_2_A Short Inter D...A Contact O3W' .. O3W = 2.03 Ang.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT301_ALERT_3_C Main Residue Disorder ......................... 1.00 Perc. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 5 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O1W -H1W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O1W -H1W2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O2W -H2W1 1.555 1.555 PLAT745_ALERT_1_C D-H Calc 0.85(3), Rep 0.85000 ...... Missing su O1W -H1W1 1.555 1.555 PLAT745_ALERT_1_C D-H Calc 0.85(3), Rep 0.85000 ...... Missing su O1W -H1W2 1.555 1.555 PLAT745_ALERT_1_C D-H Calc 0.85(2), Rep 0.84000 ...... Missing su O2W -H2W2 1.555 1.555 PLAT745_ALERT_1_C D-H Calc 0.85(3), Rep 0.85000 ...... Missing su O2W -H2W1 1.555 1.555 PLAT746_ALERT_1_C H...A Calc 2.07(3), Rep 2.07000 ...... Missing su H1W1 -O1 1.555 2.665 PLAT746_ALERT_1_C H...A Calc 2.04(2), Rep 2.04000 ...... Missing su H2W2 -O2 1.555 1.565 PLAT746_ALERT_1_C H...A Calc 1.96(3), Rep 1.96000 ...... Missing su H2W1 -O3 1.555 1.555 PLAT748_ALERT_1_C D-H..A Calc 153(5), Rep 152.00 ...... Missing su O2W -H2W1 -O3 1.555 1.555 1.555
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C10 H14 Ni2 O14 Atom count from the _atom_site data: C10 H10 Ni2 O14 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 1 From the CIF: _chemical_formula_sum C10 H14 Ni2 O14 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 10.00 10.00 0.00 H 14.00 10.00 4.00 Ni 2.00 2.00 0.00 O 14.00 14.00 0.00
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 19 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 18 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 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CAD-4 Software (Enraf-Nonius Delft, 1988); cell refinement: CAD-4 Software; data reduction: XCAD4/PC (Harms, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-II (Johnson, 1976); software used to prepare material for publication: SHELXL97.

catena-[µ6-1,2,4,5-Benzenetetracarboxylato-tetraaqua-dinickel(II)] dihydrate top
Crystal data top
[Ni2(C10H2O8·(H2O)4]2H2OZ = 1
Mr = 475.63F(000) = 242
Triclinic, P1Dx = 2.003 Mg m3
a = 6.910 (1) ÅMo Kα radiation, λ = 0.71073 Å
b = 7.389 (1) ÅCell parameters from 25 reflections
c = 8.223 (1) Åθ = 12.0–15.0°
α = 90.08 (7)°µ = 2.47 mm1
β = 109.83 (8)°T = 298 K
γ = 93.37 (7)°Prism, green
V = 394.2 (1) Å30.18 × 0.11 × 0.11 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
1594 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.031
Graphite monochromatorθmax = 30.0°, θmin = 2.6°
ω scanh = 09
Absorption correction: psi scan
(North et al., 1968)
k = 1010
Tmin = 0.674, Tmax = 0.758l = 1110
2476 measured reflections2 standard reflections every 60 min
2300 independent reflections intensity decay: none
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)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.0438P)2 + 0.0381P]
where P = (Fo2 + 2Fc2)/3
2300 reflections(Δ/σ)max = 0.001
136 parametersΔρmax = 1.06 e Å3
6 restraintsΔρmin = 0.83 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni10.00000.50000.00000.0126 (2)
Ni20.50001.00000.00000.0106 (2)
O10.5524 (4)0.2356 (3)0.1490 (3)0.0152 (5)
O20.2549 (4)0.3621 (4)0.0385 (3)0.0206 (6)
O30.1707 (4)0.7297 (3)0.1046 (3)0.0182 (6)
O40.4875 (4)0.8589 (4)0.2103 (3)0.0206 (6)
O1w0.0415 (5)0.5832 (5)0.2315 (4)0.0265 (7)
O2w0.1856 (4)1.0133 (4)0.1066 (4)0.0192 (6)
O3w0.149 (1)0.041 (1)0.520 (1)0.047 (1)0.50
O3w'0.096 (1)0.278 (1)0.423 (1)0.047 (1)0.50
C10.4190 (6)0.3387 (5)0.1597 (5)0.0121 (7)
C20.4605 (6)0.4286 (5)0.3332 (4)0.0118 (7)
C30.4188 (5)0.6079 (5)0.3572 (5)0.0121 (7)
C40.4579 (6)0.6770 (5)0.5226 (5)0.0124 (7)
C50.3524 (6)0.7395 (5)0.2120 (4)0.0131 (7)
H1w10.149 (4)0.648 (5)0.228 (6)0.032*
H1w20.039 (7)0.483 (3)0.283 (6)0.032*
H2w10.138 (7)0.930 (3)0.057 (5)0.023*
H2w20.154 (7)1.116 (2)0.081 (5)0.023*
H40.42900.79600.53750.015*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0109 (4)0.0119 (3)0.0123 (4)0.0016 (3)0.0004 (3)0.0008 (3)
Ni20.0120 (4)0.0097 (3)0.0087 (3)0.0010 (3)0.0019 (3)0.0008 (2)
O10.012 (1)0.017 (1)0.015 (1)0.005 (1)0.001 (1)0.005 (1)
O20.016 (1)0.026 (2)0.015 (1)0.008 (1)0.003 (1)0.005 (1)
O30.015 (1)0.016 (1)0.018 (1)0.000 (1)0.001 (1)0.004 (1)
O40.020 (2)0.024 (1)0.013 (1)0.007 (1)0.001 (1)0.007 (1)
O1w0.022 (2)0.038 (2)0.017 (2)0.006 (1)0.005 (1)0.002 (1)
O2w0.014 (1)0.018 (1)0.024 (2)0.003 (1)0.005 (1)0.001 (1)
O3w0.043 (3)0.048 (3)0.036 (3)0.006 (3)0.003 (2)0.010 (2)
O3w'0.043 (3)0.048 (3)0.036 (3)0.006 (3)0.003 (2)0.010 (2)
C10.016 (2)0.011 (2)0.011 (2)0.001 (1)0.005 (1)0.000 (1)
C20.016 (2)0.012 (2)0.009 (2)0.001 (1)0.006 (1)0.001 (1)
C30.011 (2)0.011 (2)0.011 (2)0.000 (1)0.001 (1)0.001 (1)
C40.014 (2)0.009 (2)0.013 (2)0.001 (1)0.003 (1)0.000 (1)
C50.017 (2)0.012 (2)0.009 (2)0.003 (1)0.003 (1)0.001 (1)
Geometric parameters (Å, º) top
Ni1—O22.018 (3)O3—C51.264 (5)
Ni1—O2i2.018 (3)O4—C51.250 (4)
Ni1—O32.021 (3)C1—C21.502 (5)
Ni1—O3i2.021 (3)C2—C4v1.391 (5)
Ni1—O1w2.106 (3)C2—C31.400 (5)
Ni1—O1wi2.106 (3)C3—C41.384 (5)
Ni2—O1ii2.069 (3)C3—C51.505 (5)
Ni2—O1iii2.069 (3)C4—C2v1.391 (5)
Ni2—O42.045 (3)O1w—H1w10.85 (1)
Ni2—O4iv2.045 (3)O1w—H1w20.85 (1)
Ni2—O2w2.057 (3)O2w—H2w10.85 (1)
Ni2—O2wiv2.057 (3)O2w—H2w20.85 (1)
O1—C11.255 (4)C4—H40.93
O2—C11.251 (5)
O2—Ni1—O2i180.0O4iv—Ni2—O2wiv94.3 (1)
O2—Ni1—O391.7 (1)O2w—Ni2—O2wiv180.0
O2—Ni1—O3i88.3 (1)C1—O1—Ni2vi126.6 (2)
O2—Ni1—O1w85.5 (1)C1—O2—Ni1137.4 (3)
O2—Ni1—O1wi94.5 (1)C5—O3—Ni1126.3 (2)
O2i—Ni1—O388.3 (1)C5—O4—Ni2126.3 (3)
O2i—Ni1—O3i91.7 (1)O2—C1—O1123.8 (3)
O2i—Ni1—O1w94.5 (1)O2—C1—C2120.2 (3)
O2i—Ni1—O1wi85.5 (1)O1—C1—C2116.0 (3)
O3i—Ni1—O3180.0 (2)C4v—C2—C3119.0 (3)
O3—Ni1—O1w85.2 (1)C4v—C2—C1116.7 (3)
O3i—Ni1—O1w94.8 (1)C3—C2—C1124.3 (3)
O3—Ni1—O1wi94.8 (1)C4—C3—C2119.9 (3)
O3i—Ni1—O1wi85.2 (1)C4—C3—C5116.6 (3)
O1w—Ni1—O1wi180.0 (2)C2—C3—C5123.2 (3)
O1ii—Ni2—O1iii180.0C3—C4—C2v121.1 (3)
O1ii—Ni2—O488.3 (1)O4—C5—O3123.8 (3)
O1ii—Ni2—O4iv91.7 (1)O4—C5—C3115.0 (3)
O1ii—Ni2—O2wiv83.8 (1)O3—C5—C3121.2 (3)
O1ii—Ni2—O2w96.2 (1)Ni1—O1w—H1w1120 (3)
O1iii—Ni2—O491.7 (1)Ni1—O1w—H1w2102 (3)
O1iii—Ni2—O4iv88.3 (1)H1w1—O1w—H1w2109 (2)
O1iii—Ni2—O2w83.8 (1)Ni2—O2w—H2w1104 (3)
O1iii—Ni2—O2wiv96.2 (1)Ni2—O2w—H2w2109 (3)
O4—Ni2—O4iv180.0 (2)H2w1—O2w—H2w2110 (2)
O4—Ni2—O2w94.3 (1)C3—C4—H4119.5
O4—Ni2—O2wiv85.7 (1)C2v—C4—H4119.5
O4iv—Ni2—O2w85.7 (1)
O3i—Ni1—O2—C1131.1 (4)O1—C1—C2—C4v40.3 (5)
O3—Ni1—O2—C148.9 (4)O2—C1—C2—C342.2 (5)
O1w—Ni1—O2—C1134.0 (4)O1—C1—C2—C3140.9 (4)
O1wi—Ni1—O2—C146.0 (4)C4v—C2—C3—C40.4 (6)
O2—Ni1—O3—C524.6 (3)C1—C2—C3—C4178.3 (3)
O2i—Ni1—O3—C5155.4 (3)C4v—C2—C3—C5173.2 (3)
O1w—Ni1—O3—C5110.0 (3)C1—C2—C3—C58.1 (6)
O1wi—Ni1—O3—C570.0 (3)C2—C3—C4—C2v0.4 (6)
O2wiv—Ni2—O4—C5143.8 (3)C5—C3—C4—C2v173.6 (3)
O2w—Ni2—O4—C536.2 (3)Ni2—O4—C5—O325.4 (5)
O1ii—Ni2—O4—C5132.3 (3)Ni2—O4—C5—C3156.5 (2)
O1iii—Ni2—O4—C547.7 (3)Ni1—O3—C5—O4142.0 (3)
Ni1—O2—C1—O1176.9 (3)Ni1—O3—C5—C340.1 (5)
Ni1—O2—C1—C20.2 (6)C4—C3—C5—O467.5 (5)
Ni2vi—O1—C1—O231.0 (5)C2—C3—C5—O4106.3 (4)
Ni2vi—O1—C1—C2145.8 (3)C4—C3—C5—O3110.6 (4)
O2—C1—C2—C4v136.6 (4)C2—C3—C5—O375.6 (5)
Symmetry codes: (i) x, y+1, z; (ii) x, y+1, z; (iii) x+1, y+1, z; (iv) x+1, y+2, z; (v) x+1, y+1, z+1; (vi) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O1iii0.852.072.897 (4)162
O1w—H1w2···O3w0.852.042.865 (9)164
O2w—H2w2···O2ii0.842.042.785 (4)147
O2w—H2w1···O30.851.962.743 (4)152
Symmetry codes: (ii) x, y+1, z; (iii) x+1, y+1, z.
 

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