Buy article online - an online subscription or single-article purchase is required to access this article.
In the title compound, [Ni(H
2O)
6](C
6H
4NO
3)
2, the Ni
II atom lies on a special position of 2/
m site symmetry in an octahedron made up of water molecules. The anions show orientational disorder over mirror planes and are linked together by a pair of N—H
O hydrogen bonds into a dianion. The complex cations and dianions are connected through O—H
O hydrogen bonds to form a three-dimensional network.
Supporting information
CCDC reference: 274605
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (i-O) = 0.003 Å
- Disorder in main residue
- R factor = 0.041
- wR factor = 0.111
- Data-to-parameter ratio = 8.6
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Ni1
PLAT301_ALERT_3_B Main Residue Disorder ......................... 29.00 Perc.
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.519 0.794
Tmin' and Tmax expected: 0.664 0.785
RR' = 0.773
Please check that your absorption correction is appropriate.
REFLT03_ALERT_3_C Reflection count < 95% complete
From the CIF: _diffrn_reflns_theta_max 27.50
From the CIF: _diffrn_reflns_theta_full 27.50
From the CIF: _reflns_number_total 974
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 1030
Completeness (_total/calc) 94.56%
PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.95
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.76
PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.62
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.06
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O1W -H1W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O2W -H2W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Rat
O2W -H2W2 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O1W -H1# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O2W -H3# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O2W -H3# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Rat
O2W -H4# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Rat
O2W -H4# 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.83(3), Rep 1.830(10) ...... 3.00 su-Rat
H1# -O1 1.555 1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.13 Ratio
0 ALERT level A = In general: serious problem
3 ALERT level B = Potentially serious problem
19 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
11 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
7 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: atomic coordinates taken from the isostructural Zn analog (Zhang et al.,
2005); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Hexaaquanickel(II) bis(6-hydroxypyridine-3-carboxylate)
top
Crystal data top
[Ni(H2O)6](C6H4NO3)2 | F(000) = 460 |
Mr = 443.01 | Dx = 1.729 Mg m−3 |
Monoclinic, C2/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1513 reflections |
a = 11.556 (1) Å | θ = 2.7–27.4° |
b = 9.767 (1) Å | µ = 1.21 mm−1 |
c = 7.5422 (8) Å | T = 295 K |
β = 91.320 (2)° | Block, light green |
V = 851.1 (2) Å3 | 0.33 × 0.28 × 0.20 mm |
Z = 2 | |
Data collection top
Bruker APEX area-detector diffractometer | 974 independent reflections |
Radiation source: fine-focus sealed tube | 939 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
φ and ω scans | θmax = 27.5°, θmin = 2.7° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −14→14 |
Tmin = 0.519, Tmax = 0.794 | k = −12→12 |
2640 measured reflections | l = −7→9 |
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)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.111 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0467P)2 + 1.687P] where P = (Fo2 + 2Fc2)/3 |
974 reflections | (Δ/σ)max = 0.001 |
113 parameters | Δρmax = 0.44 e Å−3 |
14 restraints | Δρmin = −0.30 e Å−3 |
Special details top
Refinement. A dimensionless value, 2µ*r (r = equivalent radius of crystal) of 0.39, was
used in the absorption correction step. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ni1 | 0.5000 | 0.5000 | 0.5000 | 0.0247 (2) | |
O1 | 0.8316 (2) | 0.6132 (2) | 0.6587 (4) | 0.047 (1) | |
O2 | 1.3234 (3) | 0.5755 (5) | 0.9708 (6) | 0.038 (1) | 0.50 |
O1w | 0.6252 (2) | 0.6436 (3) | 0.5003 (4) | 0.059 (1) | |
O2w | 0.4911 (3) | 0.5000 | 0.2271 (5) | 0.069 (1) | |
N1 | 1.1464 (4) | 0.6540 (6) | 0.8856 (7) | 0.037 (1) | 0.50 |
C1 | 1.0379 (5) | 0.6374 (7) | 0.8162 (7) | 0.033 (2) | 0.50 |
C2 | 1.0004 (4) | 0.510 (1) | 0.7601 (6) | 0.032 (1) | 0.50 |
C3 | 1.0769 (5) | 0.4022 (7) | 0.7772 (9) | 0.033 (2) | 0.50 |
C4 | 1.1872 (5) | 0.4178 (7) | 0.8480 (9) | 0.036 (2) | 0.50 |
C5 | 1.2241 (5) | 0.5484 (6) | 0.9041 (8) | 0.029 (1) | 0.50 |
C6 | 0.8782 (3) | 0.5000 | 0.6855 (5) | 0.030 (1) | |
H2o | 1.3246 | 0.6578 | 1.0073 | 0.046* | 0.50 |
H1w1 | 0.688 (2) | 0.623 (3) | 0.551 (5) | 0.05 (1)* | |
H1w2 | 0.626 (2) | 0.7228 (18) | 0.457 (4) | 0.04 (1)* | |
H2w1 | 0.429 (2) | 0.5000 | 0.167 (6) | 0.07 (2)* | |
H2w2 | 0.549 (3) | 0.5000 | 0.161 (6) | 0.06 (2)* | |
H1 | 0.9885 | 0.7123 | 0.8064 | 0.040* | 0.50 |
H3 | 1.0531 | 0.3157 | 0.7395 | 0.040* | 0.50 |
H4 | 1.2365 | 0.3429 | 0.8586 | 0.043* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0177 (3) | 0.0296 (4) | 0.0264 (4) | 0.000 | −0.0046 (2) | 0.000 |
O1 | 0.043 (1) | 0.035 (1) | 0.062 (2) | 0.0030 (9) | −0.023 (1) | 0.008 (1) |
O2 | 0.022 (2) | 0.051 (2) | 0.040 (3) | −0.002 (2) | −0.010 (2) | −0.005 (2) |
O1w | 0.031 (1) | 0.044 (1) | 0.099 (2) | −0.012 (1) | −0.028 (1) | 0.031 (1) |
O2w | 0.033 (2) | 0.150 (4) | 0.025 (2) | 0.000 | −0.006 (1) | 0.000 |
N1 | 0.028 (2) | 0.037 (3) | 0.044 (3) | −0.001 (2) | −0.017 (2) | 0.000 (2) |
C1 | 0.027 (4) | 0.037 (4) | 0.036 (4) | 0.001 (3) | −0.013 (3) | 0.000 (3) |
C2 | 0.025 (2) | 0.045 (4) | 0.025 (2) | 0.012 (6) | −0.006 (2) | 0.008 (5) |
C3 | 0.028 (4) | 0.035 (4) | 0.037 (4) | 0.003 (3) | −0.002 (3) | −0.006 (3) |
C4 | 0.030 (4) | 0.031 (4) | 0.047 (5) | 0.000 (3) | −0.005 (3) | −0.006 (3) |
C5 | 0.025 (3) | 0.031 (3) | 0.032 (4) | 0.004 (2) | −0.002 (2) | 0.001 (2) |
C6 | 0.029 (2) | 0.034 (2) | 0.027 (2) | 0.000 | −0.008 (2) | 0.000 |
Geometric parameters (Å, º) top
Ni1—O1w | 2.015 (2) | C3—C4 | 1.379 (7) |
Ni1—O1wi | 2.015 (2) | C4—C5 | 1.408 (7) |
Ni1—O1wii | 2.015 (2) | C6—O1iii | 1.244 (3) |
Ni1—O1wiii | 2.015 (2) | C6—C2iii | 1.512 (6) |
Ni1—O2w | 2.059 (4) | O2—H2O | 0.85 |
Ni1—O2wii | 2.059 (4) | O1w—H1w1 | 0.84 (1) |
O1—C6 | 1.244 (3) | O1w—H1w2 | 0.84 (1) |
O2—C5 | 1.270 (7) | O2w—H2w1 | 0.84 (1) |
N1—C1 | 1.357 (7) | O2w—H2w2 | 0.84 (1) |
N1—C5 | 1.372 (6) | C1—H1 | 0.93 |
C1—C2 | 1.379 (9) | C3—H3 | 0.93 |
C2—C3 | 1.380 (8) | C4—H4 | 0.93 |
C2—C6 | 1.512 (6) | | |
| | | |
O1wii—Ni1—O1w | 180 | C3—C4—C5 | 119.2 (6) |
O1wii—Ni1—O1wiii | 91.8 (2) | O2—C5—N1 | 117.8 (5) |
O1w—Ni1—O1wiii | 88.2 (2) | O2—C5—C4 | 124.9 (5) |
O1wii—Ni1—O1wi | 88.2 (2) | N1—C5—C4 | 117.2 (6) |
O1w—Ni1—O1wi | 91.8 (2) | O1iii—C6—O1 | 125.4 (4) |
O1wiii—Ni1—O1wi | 180 | O1iii—C6—C2iii | 113.5 (5) |
O1wii—Ni1—O2wii | 91.2 (1) | O1—C6—C2iii | 121.1 (5) |
O1w—Ni1—O2wii | 88.8 (1) | O1iii—C6—C2 | 121.1 (5) |
O1wiii—Ni1—O2wii | 88.8 (1) | O1—C6—C2 | 113.5 (5) |
O1wi—Ni1—O2wii | 91.2 (1) | Ni1—O1w—H1w1 | 117 (2) |
O1wii—Ni1—O2w | 88.8 (1) | Ni1—O1w—H1w2 | 131 (2) |
O1w—Ni1—O2w | 91.2 (1) | H1w1—O1w—H1w2 | 112 (2) |
O1wiii—Ni1—O2w | 91.2 (1) | Ni1—O2w—H2w1 | 124 (4) |
O1wi—Ni1—O2w | 88.8 (1) | Ni1—O2w—H2w2 | 125 (4) |
O2wii—Ni1—O2w | 180 | H2w1—O2w—H2w2 | 111 (2) |
C1—N1—C5 | 123.1 (6) | N1—C1—H1 | 119.8 |
N1—C1—C2 | 120.5 (6) | C2—C1—H1 | 119.8 |
C3—C2—C1 | 117.6 (5) | C4—C3—H3 | 118.8 |
C3—C2—C6 | 125.1 (8) | C2—C3—H3 | 118.8 |
C1—C2—C6 | 117.2 (7) | C3—C4—H4 | 120.4 |
C4—C3—C2 | 122.4 (6) | C5—C4—H4 | 120.4 |
| | | |
C5—N1—C1—C2 | 0.0 (3) | C3—C4—C5—O2 | −179.9 (6) |
N1—C1—C2—C3 | −0.1 (3) | C3—C4—C5—N1 | 0.4 (7) |
N1—C1—C2—C6 | 179.6 (4) | C3—C2—C6—O1iii | 11.3 (7) |
C1—C2—C3—C4 | 0.3 (6) | C1—C2—C6—O1iii | −168.4 (4) |
C6—C2—C3—C4 | −179.4 (5) | C3—C2—C6—O1 | −169.9 (4) |
C2—C3—C4—C5 | −0.5 (8) | C1—C2—C6—O1 | 10.4 (5) |
C1—N1—C5—O2 | −180.0 (5) | C3—C2—C6—C2iii | 10.7 (4) |
C1—N1—C5—C4 | −0.2 (6) | C1—C2—C6—C2iii | −169.0 (3) |
Symmetry codes: (i) −x+1, y, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O1 | 0.84 (1) | 1.83 (1) | 2.659 (3) | 169 (3) |
O1w—H1w2···O1iv | 0.84 (1) | 1.90 (1) | 2.713 (3) | 164 (3) |
O2w—H2w1···O2v | 0.84 (1) | 2.03 (2) | 2.804 (5) | 152 (3) |
O2w—H2w1···O2v | 0.84 (1) | 2.03 (2) | 2.804 (5) | 152 (3) |
O2w—H2w2···O2vi | 0.84 (1) | 1.94 (1) | 2.741 (6) | 158 (1) |
O2w—H2w2···O2vii | 0.84 (1) | 1.94 (1) | 2.741 (6) | 158 (1) |
O2—H2o···N1viii | 0.85 | 2.03 | 2.874 (7) | 170 |
Symmetry codes: (iv) −x+3/2, −y+3/2, −z+1; (v) x−1, y, z−1; (vi) −x+2, −y+1, −z+1; (vii) −x+2, y, −z+1; (viii) −x+5/2, −y+3/2, −z+2. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.