Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804032052/ac6145sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804032052/ac6145Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.003 Å
- R factor = 0.031
- wR factor = 0.091
- Data-to-parameter ratio = 13.0
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Ni - O2 .. 10.52 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Ni - N1 .. 13.87 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Ni - N2 .. 12.52 su
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Ni PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 3 N1 -NI -N1 -C3 82.00 7.00 3.655 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 4 N2 -NI -N2 -C4 -35.00 7.00 3.655 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 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
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2003); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Ni(C2H8N2)2](NO3)2 | F(000) = 316 |
Mr = 302.94 | Dx = 1.681 Mg m−3 |
Monoclinic, P21/c | Cu Kα radiation, λ = 1.54178 Å |
Hall symbol: -P 2ybc | Cell parameters from 2387 reflections |
a = 8.2382 (2) Å | θ = 4.4–65.0° |
b = 10.0125 (3) Å | µ = 2.67 mm−1 |
c = 7.8277 (2) Å | T = 150 K |
β = 111.998 (1)° | Plate, pale purple |
V = 598.66 (3) Å3 | 0.29 × 0.11 × 0.01 mm |
Z = 2 |
Bruker SMART 6000 CCD diffractometer | 926 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.026 |
ω scans | θmax = 67.0°, θmin = 5.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | h = −9→8 |
Tmin = 0.512, Tmax = 0.974 | k = −11→9 |
3389 measured reflections | l = −9→8 |
1027 independent reflections |
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)] = 0.031 | Hydrogen site location: mixed |
wR(F2) = 0.092 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0595P)2 + 0.1767P] where P = (Fo2 + 2Fc2)/3 |
1027 reflections | (Δ/σ)max < 0.001 |
79 parameters | Δρmax = 0.38 e Å−3 |
0 restraints | Δρmin = −0.27 e Å−3 |
Experimental. The crystal was mounted in a Cryo-loop with Paratone-N. The final unit cell is obtained from the refinement of the XYZ weighted centroids of reflections above 20 σ(I). Note that the absorption correction parameters Tmin and Tmax also reflect beam corrections, etc. As a result, the numerical values for Tmin and Tmax may differ from expected values based solely on absorption effects and crystal size. |
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. |
x | y | z | Uiso*/Ueq | ||
Ni | 0.5000 | 0.0000 | 0.0000 | 0.0172 (2) | |
N1 | 0.6621 (2) | 0.15537 (18) | 0.0206 (3) | 0.0328 (4) | |
H1A | 0.6860 | 0.1620 | −0.0849 | 0.039* | |
H1B | 0.6101 | 0.2336 | 0.0350 | 0.039* | |
N2 | 0.7099 (2) | −0.08746 (18) | 0.1871 (2) | 0.0298 (4) | |
H2A | 0.7012 | −0.0859 | 0.3009 | 0.036* | |
H2B | 0.7168 | −0.1751 | 0.1551 | 0.036* | |
C3 | 0.8260 (3) | 0.1333 (2) | 0.1815 (4) | 0.0439 (6) | |
H3A | 0.8117 | 0.1638 | 0.2954 | 0.053* | |
H3B | 0.9228 | 0.1846 | 0.1670 | 0.053* | |
C4 | 0.8675 (4) | −0.0141 (2) | 0.1942 (4) | 0.0383 (6) | |
H4A | 0.9010 | −0.0416 | 0.0905 | 0.046* | |
H4B | 0.9663 | −0.0338 | 0.3110 | 0.046* | |
N3 | 0.3284 (2) | 0.05798 (19) | 0.3331 (2) | 0.0289 (4) | |
O1 | 0.2690 (2) | 0.12956 (16) | 0.4279 (2) | 0.0390 (4) | |
O2 | 0.4085 (2) | 0.11111 (16) | 0.2437 (2) | 0.0400 (4) | |
O3 | 0.3045 (2) | −0.06558 (16) | 0.3278 (2) | 0.0408 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni | 0.0233 (3) | 0.0102 (3) | 0.0182 (3) | 0.00025 (15) | 0.0080 (2) | 0.00177 (14) |
N1 | 0.0416 (11) | 0.0208 (9) | 0.0370 (10) | 0.0001 (8) | 0.0160 (8) | −0.0003 (7) |
N2 | 0.0377 (10) | 0.0249 (9) | 0.0274 (9) | 0.0021 (7) | 0.0129 (7) | 0.0008 (7) |
C3 | 0.0402 (14) | 0.0293 (13) | 0.0540 (15) | −0.0053 (10) | 0.0083 (11) | −0.0047 (11) |
C4 | 0.0362 (13) | 0.0319 (13) | 0.0441 (14) | 0.0015 (9) | 0.0119 (11) | −0.0009 (9) |
N3 | 0.0377 (11) | 0.0230 (10) | 0.0245 (9) | 0.0006 (8) | 0.0101 (8) | 0.0008 (7) |
O1 | 0.0578 (11) | 0.0300 (9) | 0.0368 (9) | 0.0050 (7) | 0.0264 (8) | −0.0006 (7) |
O2 | 0.0584 (11) | 0.0305 (9) | 0.0420 (9) | −0.0067 (7) | 0.0312 (8) | −0.0036 (7) |
O3 | 0.0599 (11) | 0.0210 (9) | 0.0448 (10) | −0.0020 (8) | 0.0235 (8) | 0.0015 (7) |
Ni—N2 | 2.0015 (18) | N2—H2B | 0.9200 |
Ni—N2i | 2.0015 (18) | C3—C4 | 1.510 (3) |
Ni—N1 | 2.0171 (18) | C3—H3A | 0.9900 |
Ni—N1i | 2.0171 (18) | C3—H3B | 0.9900 |
N1—C3 | 1.478 (3) | C4—H4A | 0.9900 |
N1—H1A | 0.9200 | C4—H4B | 0.9900 |
N1—H1B | 0.9200 | N3—O2 | 1.247 (2) |
N2—C4 | 1.474 (3) | N3—O3 | 1.251 (3) |
N2—H2A | 0.9200 | N3—O1 | 1.255 (2) |
N2—Ni—N2i | 180.0 | H2A—N2—H2B | 108.4 |
N2—Ni—N1 | 85.08 (7) | N1—C3—C4 | 108.30 (19) |
N2i—Ni—N1 | 94.92 (7) | N1—C3—H3A | 110.0 |
N2—Ni—N1i | 94.92 (7) | C4—C3—H3A | 110.0 |
N2i—Ni—N1i | 85.08 (7) | N1—C3—H3B | 110.0 |
N1—Ni—N1i | 180.0 | C4—C3—H3B | 110.0 |
C3—N1—Ni | 108.60 (14) | H3A—C3—H3B | 108.4 |
C3—N1—H1A | 110.0 | N2—C4—C3 | 108.1 (2) |
Ni—N1—H1A | 110.0 | N2—C4—H4A | 110.1 |
C3—N1—H1B | 110.0 | C3—C4—H4A | 110.1 |
Ni—N1—H1B | 110.0 | N2—C4—H4B | 110.1 |
H1A—N1—H1B | 108.3 | C3—C4—H4B | 110.1 |
C4—N2—Ni | 108.47 (14) | H4A—C4—H4B | 108.4 |
C4—N2—H2A | 110.0 | O2—N3—O3 | 120.85 (17) |
Ni—N2—H2A | 110.0 | O2—N3—O1 | 119.59 (18) |
C4—N2—H2B | 110.0 | O3—N3—O1 | 119.55 (16) |
Ni—N2—H2B | 110.0 | ||
N2—Ni—N1—C3 | −11.64 (15) | N1i—Ni—N2—C4 | 163.78 (15) |
N2i—Ni—N1—C3 | 168.36 (15) | Ni—N1—C3—C4 | 36.6 (2) |
N1i—Ni—N1—C3 | 82 (7) | Ni—N2—C4—C3 | 40.4 (2) |
N2i—Ni—N2—C4 | −35 (7) | N1—C3—C4—N2 | −51.2 (3) |
N1—Ni—N2—C4 | −16.22 (15) |
Symmetry code: (i) −x+1, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O3i | 0.92 | 2.16 | 2.980 (3) | 148 |
N1—H1B···O3ii | 0.92 | 2.26 | 3.008 (2) | 138 |
N2—H2A···O1iii | 0.92 | 2.09 | 2.983 (2) | 163 |
N2—H2B···O1iv | 0.92 | 2.08 | 2.998 (2) | 178 |
Symmetry codes: (i) −x+1, −y, −z; (ii) −x+1, y+1/2, −z+1/2; (iii) −x+1, −y, −z+1; (iv) −x+1, y−1/2, −z+1/2. |