The title compound, [Ni(C12H8N2)(H2O)4](C10H6S2O6)·2H2O, is isostructural with a copper(II) analog, whose structure has been reported recently [Liu, Fan & Li (2006). Acta Cryst. E62, m2165–m2166]. The cation lies on a crystallographic twofold rotation axis and the anion lies on a centre of inversion. The NiII atom is in a distorted octahedral geometry.
Supporting information
CCDC reference: 1195208
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (C-C) = 0.004 Å
- R factor = 0.036
- wR factor = 0.096
- Data-to-parameter ratio = 14.0
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D H2WB .. H3WA .. 1.96 Ang.
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.84
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3WA .. O1W .. 2.61 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Ra
O2W -H2WB 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Ra
O2W -H2WA 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 111.8(7), Rep 111.8(3) ...... 2.33 su-Ra
H3WA -O3W -H3WB 1.555 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Ra
O2W -H3# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Ra
O2W -H4# 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.86(4), Rep 1.860(10) ...... 4.00 su-Ra
H3# -O3W 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.91(3), Rep 1.910(10) ...... 3.00 su-Ra
H4# -O3 1.555 7.666
Alert level G
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 0.841
Tmax scaled 0.841 Tmin scaled 0.750
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
11 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
8 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
3 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97; molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.
Tetraaqua(1,10-phenanthroline-
κ2N,
N')nickel(II)
naphthalene-1,5-disulfonate dihydrate
top
Crystal data top
[Ni(C12H8N2)(H2O)4](C10H6O6S2)·2H2O | F(000) = 1312 |
Mr = 633.28 | Dx = 1.594 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 3328 reflections |
a = 20.562 (3) Å | θ = 3.3–26.3° |
b = 12.4311 (19) Å | µ = 0.96 mm−1 |
c = 12.5373 (18) Å | T = 294 K |
β = 124.576 (2)° | Block, green |
V = 2638.6 (7) Å3 | 0.20 × 0.20 × 0.18 mm |
Z = 4 | |
Data collection top
Bruker SMART APEX CCD area-detector diffractometer | 2677 independent reflections |
Radiation source: fine-focus sealed tube | 2167 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
φ and ω scans | θmax = 26.4°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −25→25 |
Tmin = 0.891, Tmax = 1.000 | k = −15→15 |
7257 measured reflections | l = −11→15 |
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)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.096 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0502P)2 + 1.2664P] where P = (Fo2 + 2Fc2)/3 |
2677 reflections | (Δ/σ)max = 0.001 |
191 parameters | Δρmax = 0.81 e Å−3 |
7 restraints | Δρmin = −0.42 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 | 0.5000 | 0.70910 (3) | 0.2500 | 0.02919 (15) | |
S1 | 0.78658 (4) | 0.52225 (4) | 0.53488 (6) | 0.03206 (17) | |
N1 | 0.53889 (11) | 0.58109 (15) | 0.37819 (18) | 0.0284 (4) | |
C1 | 0.58062 (15) | 0.5823 (2) | 0.5073 (2) | 0.0398 (6) | |
H1A | 0.5934 | 0.6482 | 0.5497 | 0.048* | |
C2 | 0.60588 (16) | 0.4878 (3) | 0.5813 (3) | 0.0507 (8) | |
H2A | 0.6353 | 0.4918 | 0.6712 | 0.061* | |
C3 | 0.58759 (17) | 0.3913 (3) | 0.5224 (3) | 0.0497 (7) | |
H3A | 0.6034 | 0.3285 | 0.5713 | 0.060* | |
C4 | 0.5212 (2) | 0.2874 (2) | 0.3150 (3) | 0.0608 (9) | |
H4A | 0.5358 | 0.2223 | 0.3593 | 0.073* | |
C5 | 0.54443 (15) | 0.3860 (2) | 0.3866 (3) | 0.0408 (6) | |
C6 | 0.52159 (13) | 0.48456 (18) | 0.3191 (2) | 0.0288 (5) | |
C7 | 0.77596 (13) | 0.38808 (17) | 0.5728 (2) | 0.0288 (5) | |
C8 | 0.78637 (14) | 0.37008 (19) | 0.6895 (2) | 0.0346 (5) | |
H8A | 0.8006 | 0.4266 | 0.7474 | 0.042* | |
C9 | 0.77563 (15) | 0.26613 (19) | 0.7220 (2) | 0.0367 (6) | |
H9A | 0.7824 | 0.2545 | 0.8010 | 0.044* | |
C10 | 0.74449 (14) | 0.31683 (19) | 0.3610 (2) | 0.0325 (5) | |
H10A | 0.7515 | 0.3848 | 0.3381 | 0.039* | |
C11 | 0.75524 (13) | 0.30251 (16) | 0.4827 (2) | 0.0275 (5) | |
O1 | 0.80171 (12) | 0.58955 (13) | 0.64160 (19) | 0.0442 (5) | |
O1W | 0.61282 (10) | 0.71732 (13) | 0.28818 (18) | 0.0344 (4) | |
H1WA | 0.6418 (13) | 0.6630 (15) | 0.325 (2) | 0.041* | |
H1WB | 0.6376 (15) | 0.7760 (13) | 0.309 (3) | 0.041* | |
O2 | 0.71284 (12) | 0.54841 (14) | 0.41342 (19) | 0.0498 (5) | |
O2W | 0.53510 (12) | 0.81917 (17) | 0.3953 (2) | 0.0578 (6) | |
H2WB | 0.5042 (16) | 0.846 (3) | 0.412 (3) | 0.069* | |
H2WA | 0.5673 (16) | 0.8709 (19) | 0.416 (3) | 0.069* | |
O3 | 0.85322 (12) | 0.52107 (15) | 0.5239 (2) | 0.0530 (5) | |
O3W | 0.42608 (19) | 0.9130 (2) | 0.4190 (3) | 0.1019 (10) | |
H3WA | 0.3969 (2) | 0.8641 (4) | 0.3689 (4) | 0.121* | |
H3WB | 0.4095 (2) | 0.9381 (3) | 0.4631 (4) | 0.121* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0283 (2) | 0.0227 (2) | 0.0371 (3) | 0.000 | 0.0188 (2) | 0.000 |
S1 | 0.0368 (3) | 0.0199 (3) | 0.0410 (4) | −0.0036 (2) | 0.0229 (3) | −0.0029 (2) |
N1 | 0.0257 (10) | 0.0345 (11) | 0.0249 (10) | −0.0036 (8) | 0.0142 (9) | −0.0024 (8) |
C1 | 0.0319 (13) | 0.0560 (16) | 0.0286 (13) | −0.0071 (11) | 0.0155 (11) | −0.0047 (12) |
C2 | 0.0320 (14) | 0.087 (2) | 0.0267 (14) | 0.0016 (14) | 0.0127 (12) | 0.0150 (14) |
C3 | 0.0417 (15) | 0.0606 (19) | 0.0491 (18) | 0.0137 (13) | 0.0271 (14) | 0.0280 (15) |
C4 | 0.079 (2) | 0.0283 (15) | 0.085 (2) | 0.0091 (13) | 0.052 (2) | 0.0126 (13) |
C5 | 0.0396 (14) | 0.0389 (14) | 0.0487 (16) | 0.0062 (11) | 0.0280 (13) | 0.0135 (12) |
C6 | 0.0279 (12) | 0.0291 (12) | 0.0318 (12) | 0.0009 (9) | 0.0184 (11) | 0.0026 (9) |
C7 | 0.0255 (11) | 0.0224 (11) | 0.0353 (13) | 0.0001 (8) | 0.0154 (10) | 0.0004 (9) |
C8 | 0.0385 (13) | 0.0283 (12) | 0.0330 (13) | −0.0008 (10) | 0.0179 (11) | −0.0040 (10) |
C9 | 0.0436 (15) | 0.0344 (13) | 0.0304 (14) | 0.0019 (10) | 0.0200 (12) | 0.0034 (10) |
C10 | 0.0353 (13) | 0.0258 (11) | 0.0344 (13) | 0.0018 (9) | 0.0186 (11) | 0.0041 (10) |
C11 | 0.0227 (11) | 0.0223 (11) | 0.0313 (12) | 0.0010 (8) | 0.0116 (10) | 0.0008 (9) |
O1 | 0.0596 (12) | 0.0260 (9) | 0.0515 (12) | −0.0086 (8) | 0.0343 (10) | −0.0102 (8) |
O1W | 0.0306 (9) | 0.0241 (9) | 0.0479 (11) | 0.0002 (6) | 0.0219 (9) | 0.0011 (7) |
O2 | 0.0581 (12) | 0.0264 (9) | 0.0483 (12) | 0.0094 (8) | 0.0203 (10) | 0.0075 (8) |
O2W | 0.0489 (13) | 0.0464 (12) | 0.0940 (17) | −0.0199 (9) | 0.0501 (13) | −0.0358 (11) |
O3 | 0.0569 (13) | 0.0406 (11) | 0.0821 (16) | −0.0187 (9) | 0.0517 (13) | −0.0181 (10) |
O3W | 0.104 (2) | 0.104 (2) | 0.130 (3) | 0.0157 (18) | 0.086 (2) | −0.0268 (19) |
Geometric parameters (Å, º) top
Ni1—N1 | 2.0728 (19) | C4—H4A | 0.93 |
Ni1—O1W | 2.0882 (17) | C5—C6 | 1.410 (3) |
Ni1—O2W | 2.054 (2) | C6—C6i | 1.430 (5) |
S1—O1 | 1.4540 (18) | C7—C8 | 1.372 (3) |
S1—O2 | 1.450 (2) | C7—C11 | 1.429 (3) |
S1—O3 | 1.4525 (19) | C8—C9 | 1.410 (3) |
Ni1—O2Wi | 2.054 (2) | C8—H8A | 0.93 |
Ni1—N1i | 2.0728 (19) | C9—C10ii | 1.353 (3) |
Ni1—O1Wi | 2.0882 (17) | C9—H9A | 0.93 |
S1—C7 | 1.781 (2) | C10—C9ii | 1.353 (3) |
N1—C1 | 1.334 (3) | C10—C11 | 1.423 (3) |
N1—C6 | 1.348 (3) | C10—H10A | 0.93 |
C1—C2 | 1.401 (4) | C11—C11ii | 1.430 (4) |
C1—H1A | 0.93 | O1W—H1WA | 0.84 (1) |
C2—C3 | 1.345 (4) | O1W—H1WB | 0.84 (1) |
C2—H2A | 0.93 | O2W—H2WB | 0.84 (1) |
C3—C5 | 1.406 (4) | O2W—H2WA | 0.85 (1) |
C3—H3A | 0.93 | O3W—H3WA | 0.83 (1) |
C4—C4i | 1.343 (7) | O3W—H3WB | 0.86 (1) |
C4—C5 | 1.431 (4) | | |
| | | |
O1W—Ni1—O1Wi | 174.40 (9) | C5—C3—H3A | 120.2 |
O2W—Ni1—O1W | 88.78 (7) | C4i—C4—C5 | 121.12 (16) |
O2Wi—Ni1—O1W | 87.49 (7) | C4i—C4—H4A | 119.4 |
O2W—Ni1—O2Wi | 96.48 (15) | C5—C4—H4A | 119.4 |
O2W—Ni1—N1i | 170.34 (8) | C3—C5—C6 | 116.9 (2) |
O2W—Ni1—N1 | 92.11 (9) | C3—C5—C4 | 123.9 (2) |
N1i—Ni1—N1 | 79.69 (10) | C6—C5—C4 | 119.3 (3) |
N1i—Ni1—O1W | 96.02 (7) | N1—C6—C5 | 123.4 (2) |
N1—Ni1—O1W | 88.29 (7) | N1—C6—C6i | 117.05 (12) |
O2Wi—Ni1—N1i | 92.11 (9) | C5—C6—C6i | 119.57 (15) |
O2Wi—Ni1—N1 | 170.34 (8) | C8—C7—C11 | 121.2 (2) |
O2W—Ni1—O1Wi | 87.49 (7) | C8—C7—S1 | 117.95 (17) |
O2Wi—Ni1—O1Wi | 88.78 (7) | C11—C7—S1 | 120.86 (17) |
N1i—Ni1—O1Wi | 88.29 (7) | C7—C8—C9 | 120.2 (2) |
N1—Ni1—O1Wi | 96.02 (7) | C7—C8—H8A | 119.9 |
O2—S1—O3 | 112.53 (13) | C9—C8—H8A | 119.9 |
O2—S1—O1 | 112.80 (11) | C10ii—C9—C8 | 120.4 (2) |
O3—S1—O1 | 111.84 (11) | C10ii—C9—H9A | 119.8 |
O2—S1—C7 | 106.07 (11) | C8—C9—H9A | 119.8 |
O3—S1—C7 | 106.30 (11) | C9ii—C10—C11 | 121.6 (2) |
O1—S1—C7 | 106.73 (11) | C9ii—C10—H10A | 119.2 |
C1—N1—C6 | 117.7 (2) | C11—C10—H10A | 119.2 |
C1—N1—Ni1 | 129.16 (17) | C10—C11—C7 | 123.3 (2) |
C6—N1—Ni1 | 113.08 (15) | C10—C11—C11ii | 118.7 (3) |
N1—C1—C2 | 122.4 (3) | C7—C11—C11ii | 118.0 (3) |
N1—C1—H1A | 118.8 | Ni1—O1W—H1WA | 115.9 (19) |
C2—C1—H1A | 118.8 | Ni1—O1W—H1WB | 120.6 (19) |
C3—C2—C1 | 120.1 (3) | H1WA—O1W—H1WB | 114 (3) |
C3—C2—H2A | 120.0 | Ni1—O2W—H2WB | 123 (2) |
C1—C2—H2A | 120.0 | Ni1—O2W—H2WA | 126 (2) |
C2—C3—C5 | 119.7 (2) | H2WB—O2W—H2WA | 101 (3) |
C2—C3—H3A | 120.2 | H3WA—O3W—H3WB | 111.8 (3) |
| | | |
N1i—Ni1—N1—C1 | 177.1 (2) | C4—C5—C6—N1 | 178.2 (2) |
O1W—Ni1—N1—C1 | 80.7 (2) | C3—C5—C6—C6i | 179.2 (3) |
O1Wi—Ni1—N1—C1 | −95.8 (2) | C4—C5—C6—C6i | −2.4 (4) |
N1i—Ni1—N1—C6 | 0.59 (11) | O2—S1—C7—C8 | −123.16 (19) |
O1W—Ni1—N1—C6 | −95.84 (15) | O3—S1—C7—C8 | 116.86 (19) |
O1Wi—Ni1—N1—C6 | 87.75 (15) | O1—S1—C7—C8 | −2.7 (2) |
C6—N1—C1—C2 | −0.4 (3) | O2—S1—C7—C11 | 55.3 (2) |
Ni1—N1—C1—C2 | −176.80 (18) | O3—S1—C7—C11 | −64.7 (2) |
N1—C1—C2—C3 | −0.6 (4) | O1—S1—C7—C11 | 175.77 (18) |
C1—C2—C3—C5 | 1.3 (4) | C11—C7—C8—C9 | −0.9 (4) |
C2—C3—C5—C6 | −0.9 (4) | S1—C7—C8—C9 | 177.54 (19) |
C2—C3—C5—C4 | −179.1 (3) | C7—C8—C9—C10ii | 0.4 (4) |
C4i—C4—C5—C3 | 178.8 (4) | C9ii—C10—C11—C7 | −179.6 (2) |
C4i—C4—C5—C6 | 0.6 (6) | C9ii—C10—C11—C11ii | 0.3 (4) |
C1—N1—C6—C5 | 0.8 (3) | C8—C7—C11—C10 | −179.4 (2) |
Ni1—N1—C6—C5 | 177.76 (18) | S1—C7—C11—C10 | 2.2 (3) |
C1—N1—C6—C6i | −178.6 (2) | C8—C7—C11—C11ii | 0.7 (4) |
Ni1—N1—C6—C6i | −1.7 (3) | S1—C7—C11—C11ii | −177.7 (2) |
C3—C5—C6—N1 | −0.2 (4) | | |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) −x+3/2, −y+1/2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O2 | 0.84 (1) | 1.89 (1) | 2.727 (2) | 176 (3) |
O1W—H1WB···O1iii | 0.84 (1) | 1.96 (1) | 2.806 (2) | 178 (3) |
O2W—H2WB···O3W | 0.84 (1) | 1.86 (1) | 2.688 (3) | 170 (3) |
O2W—H2WA···O3iii | 0.85 (1) | 1.91 (1) | 2.758 (3) | 174 (4) |
O3W—H3WA···O1iv | 0.83 (1) | 2.44 (1) | 2.922 (4) | 118 (1) |
O3W—H3WA···O1Wi | 0.83 (1) | 2.61 (1) | 3.308 (3) | 142 (1) |
O3W—H3WB···O3v | 0.86 (1) | 2.00 (1) | 2.832 (3) | 165 (1) |
Symmetry codes: (i) −x+1, y, −z+1/2; (iii) −x+3/2, −y+3/2, −z+1; (iv) x−1/2, −y+3/2, z−1/2; (v) x−1/2, y+1/2, z. |