In the title complex, [Ni(H2O)6]L2·2H2O, where L is p-nitrobenzoate (C7H4NO4), each NiII cation lies on an inversion center and is octahedrally coordinated by six water molecules. The L- anions do not coordinate to the nickel, but act as counter-anions. The crystal structure is composed of alternating layers of [Ni(H2O)6]2+ cations and L anions. The [Ni(H2O)6]2+ cations, water molecules and L- anions are connected through a complex pattern of hydrogen-bonding interactions, resulting in a three-dimensional network.
Supporting information
CCDC reference: 251611
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.007 Å
- R factor = 0.053
- wR factor = 0.160
- Data-to-parameter ratio = 13.2
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors for C2
PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors for C5
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - O6 .. 8.39 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - O7 .. 7.54 su
PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for C3
PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for C6
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for Ni1
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for N1
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for C1
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 3.34
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7
PLAT480_ALERT_4_C Long H...A H-Bond Reported H5A .. O7 .. 2.62 Ang.
0 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
12 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
10 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
Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
Hexaaquanickel(II) bis(
p-nitrobenzoate) dihydrate
top
Crystal data top
[Ni(H2O)6](C7H4NO4)2·2H2O | F(000) = 1112 |
Mr = 535.06 | Dx = 1.580 Mg m−3 |
Monoclinic, C2/c | Melting point: 433 K |
Hall symbol: -C 2yc | Mo Kα radiation, λ = 0.71073 Å |
a = 29.030 (6) Å | Cell parameters from 60 reflections |
b = 7.0550 (14) Å | θ = 2.5–24.4° |
c = 11.916 (2) Å | µ = 0.94 mm−1 |
β = 112.85 (3)° | T = 293 K |
V = 2249.0 (8) Å3 | Block, light blue |
Z = 4 | 0.42 × 0.27 × 0.26 mm |
Data collection top
Siemens SMART diffractometer | 1986 independent reflections |
Radiation source: fine-focus sealed tube | 1818 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
φ and ω scans | θmax = 25.0°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −34→25 |
Tmin = 0.744, Tmax = 0.782 | k = −8→5 |
4473 measured reflections | l = −13→14 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.053 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.160 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.1011P)2 + 4.0152P] where P = (Fo2 + 2Fc2)/3 |
1986 reflections | (Δ/σ)max < 0.001 |
150 parameters | Δρmax = 0.54 e Å−3 |
0 restraints | Δρmin = −0.46 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Ni1 | 0.0000 | 0.02951 (9) | 0.2500 | 0.0362 (3) | |
N1 | 0.32598 (12) | 0.6403 (5) | 0.9123 (3) | 0.0516 (8) | |
O1 | 0.13392 (13) | 0.6545 (7) | 0.4125 (3) | 0.0951 (14) | |
O2 | 0.09600 (10) | 0.6403 (6) | 0.5404 (3) | 0.0730 (10) | |
O3 | 0.36321 (11) | 0.6421 (7) | 0.8916 (3) | 0.0881 (12) | |
O4 | 0.32782 (14) | 0.6452 (10) | 1.0143 (3) | 0.1172 (19) | |
O5 | −0.01378 (9) | −0.1893 (4) | 0.1170 (2) | 0.0463 (6) | |
H5A | 0.0098 | −0.2290 | 0.0977 | 0.080* | |
H5B | −0.0429 | −0.2367 | 0.0835 | 0.080* | |
O6 | 0.07419 (12) | 0.0217 (5) | 0.2586 (3) | 0.0681 (9) | |
H6B | 0.0819 | −0.0556 | 0.2141 | 0.080* | |
H6C | 0.0962 | 0.0956 | 0.3065 | 0.080* | |
O7 | 0.02114 (13) | 0.2325 (5) | 0.3896 (3) | 0.0713 (9) | |
H7B | 0.0503 | 0.2293 | 0.4456 | 0.080* | |
H7C | 0.0006 | 0.3181 | 0.3901 | 0.080* | |
O8 | 0.06118 (11) | 0.5394 (4) | 0.2008 (3) | 0.0599 (8) | |
H8A | 0.0680 | 0.5558 | 0.1383 | 0.080* | |
H8B | 0.0668 | 0.6274 | 0.2532 | 0.080* | |
C1 | 0.13388 (15) | 0.6396 (6) | 0.5165 (4) | 0.0507 (10) | |
C2 | 0.18449 (13) | 0.6362 (5) | 0.6223 (3) | 0.0391 (8) | |
C3 | 0.22744 (17) | 0.6343 (11) | 0.6016 (4) | 0.088 (2) | |
H3A | 0.2252 | 0.6313 | 0.5191 | 0.080* | |
C4 | 0.27409 (15) | 0.6374 (10) | 0.6952 (4) | 0.0787 (18) | |
H4A | 0.3039 | 0.6403 | 0.6787 | 0.080* | |
C5 | 0.27698 (13) | 0.6377 (5) | 0.8107 (3) | 0.0403 (8) | |
C6 | 0.23512 (17) | 0.6380 (11) | 0.8345 (4) | 0.0856 (19) | |
H6A | 0.2377 | 0.6419 | 0.9173 | 0.080* | |
C7 | 0.18860 (15) | 0.6375 (9) | 0.7394 (4) | 0.0724 (15) | |
H7A | 0.1589 | 0.6365 | 0.7564 | 0.080* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0294 (4) | 0.0453 (4) | 0.0314 (4) | 0.000 | 0.0089 (3) | 0.000 |
N1 | 0.0399 (18) | 0.056 (2) | 0.050 (2) | 0.0037 (14) | 0.0075 (15) | 0.0023 (15) |
O1 | 0.057 (2) | 0.173 (4) | 0.0427 (18) | −0.007 (2) | 0.0060 (15) | −0.009 (2) |
O2 | 0.0350 (15) | 0.113 (3) | 0.0610 (19) | 0.0018 (16) | 0.0083 (13) | 0.0342 (18) |
O3 | 0.0352 (16) | 0.148 (4) | 0.074 (2) | 0.0000 (19) | 0.0133 (15) | −0.019 (2) |
O4 | 0.056 (2) | 0.238 (6) | 0.042 (2) | 0.010 (3) | 0.0013 (16) | 0.019 (3) |
O5 | 0.0374 (13) | 0.0564 (15) | 0.0426 (14) | −0.0060 (11) | 0.0128 (11) | −0.0114 (11) |
O6 | 0.0480 (18) | 0.086 (2) | 0.070 (2) | −0.0077 (15) | 0.0220 (16) | −0.0153 (16) |
O7 | 0.070 (2) | 0.072 (2) | 0.0609 (19) | 0.0039 (17) | 0.0141 (16) | −0.0131 (16) |
O8 | 0.0428 (16) | 0.077 (2) | 0.0542 (18) | 0.0015 (13) | 0.0120 (13) | −0.0139 (14) |
C1 | 0.044 (2) | 0.054 (2) | 0.043 (2) | −0.0024 (17) | 0.0048 (17) | 0.0051 (17) |
C2 | 0.0367 (18) | 0.0373 (18) | 0.0389 (18) | −0.0010 (14) | 0.0096 (15) | 0.0011 (14) |
C3 | 0.045 (2) | 0.182 (6) | 0.037 (2) | −0.008 (3) | 0.0157 (19) | −0.025 (3) |
C4 | 0.032 (2) | 0.155 (6) | 0.050 (3) | −0.006 (3) | 0.0176 (18) | −0.028 (3) |
C5 | 0.0336 (17) | 0.0410 (19) | 0.0407 (18) | 0.0022 (14) | 0.0082 (15) | 0.0026 (14) |
C6 | 0.042 (2) | 0.179 (6) | 0.033 (2) | −0.001 (3) | 0.0128 (18) | 0.021 (3) |
C7 | 0.032 (2) | 0.139 (5) | 0.043 (2) | 0.002 (2) | 0.0124 (17) | 0.017 (3) |
Geometric parameters (Å, º) top
Ni1—O7 | 2.098 (3) | O7—H7B | 0.8501 |
Ni1—O7i | 2.098 (3) | O7—H7C | 0.8500 |
Ni1—O6i | 2.117 (3) | O8—H8A | 0.8499 |
Ni1—O6 | 2.117 (3) | O8—H8B | 0.8500 |
Ni1—O5 | 2.136 (2) | C1—C2 | 1.520 (5) |
Ni1—O5i | 2.136 (2) | C2—C7 | 1.353 (6) |
N1—O4 | 1.196 (5) | C2—C3 | 1.362 (6) |
N1—O3 | 1.198 (5) | C3—C4 | 1.380 (6) |
N1—C5 | 1.467 (5) | C3—H3A | 0.9600 |
O1—C1 | 1.245 (5) | C4—C5 | 1.346 (6) |
O2—C1 | 1.238 (5) | C4—H4A | 0.9599 |
O5—H5A | 0.8502 | C5—C6 | 1.351 (6) |
O5—H5B | 0.8499 | C6—C7 | 1.385 (6) |
O6—H6B | 0.8501 | C6—H6A | 0.9599 |
O6—H6C | 0.8500 | C7—H7A | 0.9601 |
| | | |
O7—Ni1—O7i | 93.9 (2) | Ni1—O7—H7C | 120.0 |
O7—Ni1—O6i | 92.01 (14) | H7B—O7—H7C | 120.0 |
O7i—Ni1—O6i | 90.02 (13) | H8A—O8—H8B | 120.0 |
O7—Ni1—O6 | 90.02 (13) | O2—C1—O1 | 125.0 (4) |
O7i—Ni1—O6 | 92.01 (14) | O2—C1—C2 | 117.9 (4) |
O6i—Ni1—O6 | 177.03 (18) | O1—C1—C2 | 117.0 (4) |
O7—Ni1—O5 | 173.96 (11) | C7—C2—C3 | 117.8 (4) |
O7i—Ni1—O5 | 89.54 (13) | C7—C2—C1 | 121.7 (3) |
O6i—Ni1—O5 | 92.95 (12) | C3—C2—C1 | 120.5 (4) |
O6—Ni1—O5 | 84.90 (12) | C2—C3—C4 | 122.3 (4) |
O7—Ni1—O5i | 89.54 (13) | C2—C3—H3A | 118.8 |
O7i—Ni1—O5i | 173.96 (11) | C4—C3—H3A | 118.9 |
O6i—Ni1—O5i | 84.90 (12) | C5—C4—C3 | 118.6 (4) |
O6—Ni1—O5i | 92.95 (12) | C5—C4—H4A | 120.4 |
O5—Ni1—O5i | 87.46 (14) | C3—C4—H4A | 121.0 |
O4—N1—O3 | 121.4 (4) | C4—C5—C6 | 120.7 (4) |
O4—N1—C5 | 119.0 (3) | C4—C5—N1 | 120.0 (3) |
O3—N1—C5 | 119.6 (3) | C6—C5—N1 | 119.3 (3) |
Ni1—O5—H5A | 120.1 | C5—C6—C7 | 119.9 (4) |
Ni1—O5—H5B | 119.9 | C5—C6—H6A | 119.8 |
H5A—O5—H5B | 120.0 | C7—C6—H6A | 120.2 |
Ni1—O6—H6B | 119.8 | C2—C7—C6 | 120.7 (4) |
Ni1—O6—H6C | 120.2 | C2—C7—H7A | 119.4 |
H6B—O6—H6C | 120.0 | C6—C7—H7A | 119.9 |
Ni1—O7—H7B | 120.0 | | |
Symmetry code: (i) −x, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5A···O8ii | 0.85 | 2.23 | 2.777 (4) | 122 |
O5—H5A···O7iii | 0.85 | 2.62 | 3.255 (5) | 132 |
O5—H5B···O2iv | 0.85 | 1.88 | 2.680 (4) | 156 |
O6—H6B···O3v | 0.85 | 2.46 | 3.221 (5) | 149 |
O6—H6C···O4vi | 0.85 | 2.43 | 3.193 (5) | 150 |
O7—H7B···O3vi | 0.85 | 2.58 | 3.417 (5) | 168 |
O7—H7C···O8i | 0.85 | 2.31 | 3.092 (5) | 154 |
O8—H8A···O2vii | 0.85 | 2.16 | 2.790 (4) | 131 |
O8—H8B···O1 | 0.85 | 2.14 | 2.710 (5) | 125 |
Symmetry codes: (i) −x, y, −z+1/2; (ii) x, y−1, z; (iii) x, −y, z−1/2; (iv) −x, y−1, −z+1/2; (v) −x+1/2, −y+1/2, −z+1; (vi) −x+1/2, y−1/2, −z+3/2; (vii) x, −y+1, z−1/2. |