catena-[μ₆-1,2,4,5-Benzene­tetra­carboxyl­ato-tetra­aqua-dinickel(II)] dihydrate

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.

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

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Computing details

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

Crystal data

[Ni2(C10H2O8·(H2O)4]2H2O	Z = 1
Mr = 475.63	F(000) = 242
Triclinic, P1	Dx = 2.003 Mg m^−3
a = 6.910 (1) Å	Mo Kα radiation, λ = 0.71073 Å
b = 7.389 (1) Å	Cell parameters from 25 reflections
c = 8.223 (1) Å	θ = 12.0–15.0°
α = 90.08 (7)°	µ = 2.47 mm^−1
β = 109.83 (8)°	T = 298 K
γ = 93.37 (7)°	Prism, green
V = 394.2 (1) Å^3	0.18 × 0.11 × 0.11 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	1594 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.031
Graphite monochromator	θmax = 30.0°, θmin = 2.6°
ω scan	h = 0→9
Absorption correction: psi scan (North et al., 1968)	k = −10→10
Tmin = 0.674, Tmax = 0.758	l = −11→10
2476 measured reflections	2 standard reflections every 60 min
2300 independent reflections	intensity decay: none

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.108	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0438P)^2 + 0.0381P] where P = (Fo^2 + 2Fc^2)/3
2300 reflections	(Δ/σ)max = 0.001
136 parameters	Δρmax = 1.06 e Å^−3
6 restraints	Δρmin = −0.83 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ni1	0.0000	0.5000	0.0000	0.0126 (2)
Ni2	0.5000	1.0000	0.0000	0.0106 (2)
O1	0.5524 (4)	0.2356 (3)	0.1490 (3)	0.0152 (5)
O2	0.2549 (4)	0.3621 (4)	0.0385 (3)	0.0206 (6)
O3	0.1707 (4)	0.7297 (3)	0.1046 (3)	0.0182 (6)
O4	0.4875 (4)	0.8589 (4)	0.2103 (3)	0.0206 (6)
O1w	0.0415 (5)	0.5832 (5)	−0.2315 (4)	0.0265 (7)
O2w	0.1856 (4)	1.0133 (4)	−0.1066 (4)	0.0192 (6)
O3w	0.149 (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
C1	0.4190 (6)	0.3387 (5)	0.1597 (5)	0.0121 (7)
C2	0.4605 (6)	0.4286 (5)	0.3332 (4)	0.0118 (7)
C3	0.4188 (5)	0.6079 (5)	0.3572 (5)	0.0121 (7)
C4	0.4579 (6)	0.6770 (5)	0.5226 (5)	0.0124 (7)
C5	0.3524 (6)	0.7395 (5)	0.2120 (4)	0.0131 (7)
H1w1	0.149 (4)	0.648 (5)	−0.228 (6)	0.032*
H1w2	0.039 (7)	0.483 (3)	−0.283 (6)	0.032*
H2w1	0.138 (7)	0.930 (3)	−0.057 (5)	0.023*
H2w2	0.154 (7)	1.116 (2)	−0.081 (5)	0.023*
H4	0.4290	0.7960	0.5375	0.015*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0109 (4)	0.0119 (3)	0.0123 (4)	0.0016 (3)	0.0004 (3)	0.0008 (3)
Ni2	0.0120 (4)	0.0097 (3)	0.0087 (3)	0.0010 (3)	0.0019 (3)	0.0008 (2)
O1	0.012 (1)	0.017 (1)	0.015 (1)	0.005 (1)	0.001 (1)	−0.005 (1)
O2	0.016 (1)	0.026 (2)	0.015 (1)	0.008 (1)	−0.003 (1)	−0.005 (1)
O3	0.015 (1)	0.016 (1)	0.018 (1)	0.000 (1)	−0.001 (1)	0.004 (1)
O4	0.020 (2)	0.024 (1)	0.013 (1)	−0.007 (1)	0.001 (1)	0.007 (1)
O1w	0.022 (2)	0.038 (2)	0.017 (2)	−0.006 (1)	0.005 (1)	0.002 (1)
O2w	0.014 (1)	0.018 (1)	0.024 (2)	0.003 (1)	0.005 (1)	−0.001 (1)
O3w	0.043 (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)
C1	0.016 (2)	0.011 (2)	0.011 (2)	−0.001 (1)	0.005 (1)	0.000 (1)
C2	0.016 (2)	0.012 (2)	0.009 (2)	0.001 (1)	0.006 (1)	−0.001 (1)
C3	0.011 (2)	0.011 (2)	0.011 (2)	0.000 (1)	0.001 (1)	0.001 (1)
C4	0.014 (2)	0.009 (2)	0.013 (2)	0.001 (1)	0.003 (1)	0.000 (1)
C5	0.017 (2)	0.012 (2)	0.009 (2)	0.003 (1)	0.003 (1)	−0.001 (1)

Geometric parameters (Å, º)

Ni1—O2	2.018 (3)	O3—C5	1.264 (5)
Ni1—O2^i	2.018 (3)	O4—C5	1.250 (4)
Ni1—O3	2.021 (3)	C1—C2	1.502 (5)
Ni1—O3^i	2.021 (3)	C2—C4^v	1.391 (5)
Ni1—O1w	2.106 (3)	C2—C3	1.400 (5)
Ni1—O1w^i	2.106 (3)	C3—C4	1.384 (5)
Ni2—O1^ii	2.069 (3)	C3—C5	1.505 (5)
Ni2—O1^iii	2.069 (3)	C4—C2^v	1.391 (5)
Ni2—O4	2.045 (3)	O1w—H1w1	0.85 (1)
Ni2—O4^iv	2.045 (3)	O1w—H1w2	0.85 (1)
Ni2—O2w	2.057 (3)	O2w—H2w1	0.85 (1)
Ni2—O2w^iv	2.057 (3)	O2w—H2w2	0.85 (1)
O1—C1	1.255 (4)	C4—H4	0.93
O2—C1	1.251 (5)
O2—Ni1—O2^i	180.0	O4^iv—Ni2—O2w^iv	94.3 (1)
O2—Ni1—O3	91.7 (1)	O2w—Ni2—O2w^iv	180.0
O2—Ni1—O3^i	88.3 (1)	C1—O1—Ni2^vi	126.6 (2)
O2—Ni1—O1w	85.5 (1)	C1—O2—Ni1	137.4 (3)
O2—Ni1—O1w^i	94.5 (1)	C5—O3—Ni1	126.3 (2)
O2^i—Ni1—O3	88.3 (1)	C5—O4—Ni2	126.3 (3)
O2^i—Ni1—O3^i	91.7 (1)	O2—C1—O1	123.8 (3)
O2^i—Ni1—O1w	94.5 (1)	O2—C1—C2	120.2 (3)
O2^i—Ni1—O1w^i	85.5 (1)	O1—C1—C2	116.0 (3)
O3^i—Ni1—O3	180.0 (2)	C4^v—C2—C3	119.0 (3)
O3—Ni1—O1w	85.2 (1)	C4^v—C2—C1	116.7 (3)
O3^i—Ni1—O1w	94.8 (1)	C3—C2—C1	124.3 (3)
O3—Ni1—O1w^i	94.8 (1)	C4—C3—C2	119.9 (3)
O3^i—Ni1—O1w^i	85.2 (1)	C4—C3—C5	116.6 (3)
O1w—Ni1—O1w^i	180.0 (2)	C2—C3—C5	123.2 (3)
O1^ii—Ni2—O1^iii	180.0	C3—C4—C2^v	121.1 (3)
O1^ii—Ni2—O4	88.3 (1)	O4—C5—O3	123.8 (3)
O1^ii—Ni2—O4^iv	91.7 (1)	O4—C5—C3	115.0 (3)
O1^ii—Ni2—O2w^iv	83.8 (1)	O3—C5—C3	121.2 (3)
O1^ii—Ni2—O2w	96.2 (1)	Ni1—O1w—H1w1	120 (3)
O1^iii—Ni2—O4	91.7 (1)	Ni1—O1w—H1w2	102 (3)
O1^iii—Ni2—O4^iv	88.3 (1)	H1w1—O1w—H1w2	109 (2)
O1^iii—Ni2—O2w	83.8 (1)	Ni2—O2w—H2w1	104 (3)
O1^iii—Ni2—O2w^iv	96.2 (1)	Ni2—O2w—H2w2	109 (3)
O4—Ni2—O4^iv	180.0 (2)	H2w1—O2w—H2w2	110 (2)
O4—Ni2—O2w	94.3 (1)	C3—C4—H4	119.5
O4—Ni2—O2w^iv	85.7 (1)	C2^v—C4—H4	119.5
O4^iv—Ni2—O2w	85.7 (1)
O3^i—Ni1—O2—C1	−131.1 (4)	O1—C1—C2—C4^v	−40.3 (5)
O3—Ni1—O2—C1	48.9 (4)	O2—C1—C2—C3	−42.2 (5)
O1w—Ni1—O2—C1	134.0 (4)	O1—C1—C2—C3	140.9 (4)
O1w^i—Ni1—O2—C1	−46.0 (4)	C4^v—C2—C3—C4	−0.4 (6)
O2—Ni1—O3—C5	−24.6 (3)	C1—C2—C3—C4	178.3 (3)
O2^i—Ni1—O3—C5	155.4 (3)	C4^v—C2—C3—C5	173.2 (3)
O1w—Ni1—O3—C5	−110.0 (3)	C1—C2—C3—C5	−8.1 (6)
O1w^i—Ni1—O3—C5	70.0 (3)	C2—C3—C4—C2^v	0.4 (6)
O2w^iv—Ni2—O4—C5	−143.8 (3)	C5—C3—C4—C2^v	−173.6 (3)
O2w—Ni2—O4—C5	36.2 (3)	Ni2—O4—C5—O3	−25.4 (5)
O1^ii—Ni2—O4—C5	132.3 (3)	Ni2—O4—C5—C3	156.5 (2)
O1^iii—Ni2—O4—C5	−47.7 (3)	Ni1—O3—C5—O4	142.0 (3)
Ni1—O2—C1—O1	176.9 (3)	Ni1—O3—C5—C3	−40.1 (5)
Ni1—O2—C1—C2	0.2 (6)	C4—C3—C5—O4	67.5 (5)
Ni2^vi—O1—C1—O2	−31.0 (5)	C2—C3—C5—O4	−106.3 (4)
Ni2^vi—O1—C1—C2	145.8 (3)	C4—C3—C5—O3	−110.6 (4)
O2—C1—C2—C4^v	136.6 (4)	C2—C3—C5—O3	75.6 (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, y−1, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H1w1···O1^iii	0.85	2.07	2.897 (4)	162
O1w—H1w2···O3w′	0.85	2.04	2.865 (9)	164
O2w—H2w2···O2^ii	0.84	2.04	2.785 (4)	147
O2w—H2w1···O3	0.85	1.96	2.743 (4)	152

Symmetry codes: (ii) x, y+1, z; (iii) −x+1, −y+1, −z.