Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536800020389/ya6000sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536800020389/ya6000Isup2.hkl |
CCDC reference: 155848
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.029
- wR factor = 0.075
- Data-to-parameter ratio = 10.9
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 30.00 From the CIF: _reflns_number_total 3459 Count of symmetry unique reflns 3472 Completeness (_total/calc) 99.63% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 0 Fraction of Friedel pairs measured 0.000 Are heavy atom types Z>Si present yes WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure
Prismatic brown single crystals of the title compound were grown by a slow diffusion. Into one arm of the H-double-tube glass vessel were added K2Cr2O7 (10 ml, 0.1 M water solution) and NiCl2 6H2O (10 ml, 0.1 M water solution). Into the other arm 2,2'-bipy was added (20 ml, 0.1 M in acetone). Both arms were covered by acetone and protected by parafilm to avoid acetone evaporation. The vessel was allowed to stand at room temperature. A few crystals of the compound appeared after one month. The crystals were selected and washed with some drops of cold water–ethanol (1:1) solution.
All H atoms have been generated at idealized geometries, except for those belonging to the water molecule which were located in difference syntheses, and refined isotropically using a riding model with displacement parameters set at 1.2Ueq·The residual electron-density maximum is 0.47 Å from the Ni1 atom.
Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: HELENA (Spek, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1998); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 1990); software used to prepare material for publication: PLATON.
[NiCr2O7(C10H8N2)2(H2O)] | F(000) = 4896 |
Mr = 605.07 | Dx = 1.763 Mg m−3 |
Orthorhombic, Fdd2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: F 2 -2d | Cell parameters from 25 reflections |
a = 33.958 (5) Å | θ = 12.0–18.2° |
b = 22.880 (3) Å | µ = 1.81 mm−1 |
c = 11.735 (1) Å | T = 293 K |
V = 9118 (2) Å3 | Prism, brown |
Z = 16 | 0.45 × 0.23 × 0.15 mm |
Enraf-Nonius CAD-4 diffractometer | 2927 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 30.0°, θmin = 2.7° |
ω scans | h = 0→47 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→32 |
Tmin = 0.613, Tmax = 0.762 | l = −16→0 |
3459 measured reflections | 3 standard reflections every 120 min |
3459 independent reflections | intensity decay: none |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.029 | H-atom parameters constrained |
wR(F2) = 0.075 | w = 1/[σ2(Fo2) + (0.0449P)2 + 0.7783P] where P = (Fo2 + 2Fc2)/3 |
S = 1.08 | (Δ/σ)max = 0.001 |
3459 reflections | Δρmax = 0.47 e Å−3 |
316 parameters | Δρmin = −0.28 e Å−3 |
1 restraint | Absolute structure: (Flack, 1983). No Fridel pairs. |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.07 (2) |
[NiCr2O7(C10H8N2)2(H2O)] | V = 9118 (2) Å3 |
Mr = 605.07 | Z = 16 |
Orthorhombic, Fdd2 | Mo Kα radiation |
a = 33.958 (5) Å | µ = 1.81 mm−1 |
b = 22.880 (3) Å | T = 293 K |
c = 11.735 (1) Å | 0.45 × 0.23 × 0.15 mm |
Enraf-Nonius CAD-4 diffractometer | 2927 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.000 |
Tmin = 0.613, Tmax = 0.762 | 3 standard reflections every 120 min |
3459 measured reflections | intensity decay: none |
3459 independent reflections |
R[F2 > 2σ(F2)] = 0.029 | H-atom parameters constrained |
wR(F2) = 0.075 | Δρmax = 0.47 e Å−3 |
S = 1.08 | Δρmin = −0.28 e Å−3 |
3459 reflections | Absolute structure: (Flack, 1983). No Fridel pairs. |
316 parameters | Absolute structure parameter: 0.07 (2) |
1 restraint |
x | y | z | Uiso*/Ueq | ||
Ni1 | 0.25588 (1) | 0.09675 (2) | 0.14283 (3) | 0.0284 (1) | |
Cr1 | 0.20367 (1) | −0.02439 (2) | 0.04115 (5) | 0.0286 (1) | |
Cr2 | 0.25111 (2) | −0.13232 (2) | 0.14984 (7) | 0.0424 (2) | |
O1 | 0.23561 (7) | 0.02875 (11) | 0.0404 (2) | 0.0403 (7) | |
O2 | 0.17587 (8) | −0.02053 (13) | 0.1489 (3) | 0.0495 (9) | |
O3 | 0.17684 (8) | −0.02120 (14) | −0.0749 (2) | 0.0460 (9) | |
O4 | 0.22817 (11) | −0.09131 (12) | 0.0356 (3) | 0.0583 (10) | |
O5 | 0.27291 (13) | −0.08786 (16) | 0.2335 (4) | 0.0788 (15) | |
O6 | 0.21848 (12) | −0.1695 (2) | 0.2144 (4) | 0.0793 (16) | |
O7 | 0.28208 (11) | −0.17435 (16) | 0.0877 (4) | 0.0690 (12) | |
O8 | 0.28768 (9) | 0.02981 (12) | 0.2210 (3) | 0.0498 (9) | |
N1 | 0.28594 (8) | 0.15630 (13) | 0.2407 (3) | 0.0316 (8) | |
N2 | 0.30522 (7) | 0.11169 (12) | 0.0417 (3) | 0.0327 (8) | |
N3 | 0.20643 (8) | 0.09356 (13) | 0.2439 (3) | 0.0337 (8) | |
N4 | 0.21845 (8) | 0.15257 (12) | 0.0538 (3) | 0.0341 (8) | |
C1 | 0.27398 (11) | 0.17877 (15) | 0.3397 (3) | 0.0380 (10) | |
C2 | 0.29693 (11) | 0.21599 (17) | 0.4057 (4) | 0.0447 (11) | |
C3 | 0.33377 (12) | 0.22989 (17) | 0.3668 (4) | 0.0470 (12) | |
C4 | 0.34674 (10) | 0.20709 (19) | 0.2650 (4) | 0.0461 (11) | |
C5 | 0.32259 (9) | 0.16983 (15) | 0.2027 (3) | 0.0324 (9) | |
C6 | 0.33366 (9) | 0.14291 (14) | 0.0939 (3) | 0.0331 (9) | |
C7 | 0.37086 (10) | 0.14878 (17) | 0.0439 (4) | 0.0432 (11) | |
C8 | 0.37863 (12) | 0.1224 (2) | −0.0580 (4) | 0.0504 (13) | |
C9 | 0.34898 (11) | 0.09138 (18) | −0.1117 (4) | 0.0480 (11) | |
C10 | 0.31252 (11) | 0.08739 (17) | −0.0599 (3) | 0.0401 (10) | |
C11 | 0.20256 (12) | 0.06450 (18) | 0.3416 (3) | 0.0433 (11) | |
C12 | 0.16805 (13) | 0.06398 (19) | 0.4039 (4) | 0.0533 (14) | |
C13 | 0.13607 (14) | 0.0937 (2) | 0.3630 (4) | 0.0620 (17) | |
C14 | 0.13961 (12) | 0.1241 (2) | 0.2622 (4) | 0.0527 (14) | |
C15 | 0.17513 (10) | 0.12408 (16) | 0.2046 (3) | 0.0365 (10) | |
C16 | 0.18188 (10) | 0.15614 (15) | 0.0966 (3) | 0.0345 (9) | |
C17 | 0.15272 (11) | 0.18777 (18) | 0.0412 (4) | 0.0493 (11) | |
C18 | 0.16187 (14) | 0.21594 (19) | −0.0607 (4) | 0.0537 (12) | |
C19 | 0.19928 (12) | 0.21221 (18) | −0.1028 (4) | 0.0481 (11) | |
C20 | 0.22671 (11) | 0.17984 (17) | −0.0446 (3) | 0.0422 (11) | |
H1 | 0.24900 | 0.16900 | 0.36600 | 0.0460* | |
H2 | 0.28760 | 0.23100 | 0.47410 | 0.0540* | |
H3 | 0.34990 | 0.25460 | 0.40900 | 0.0560* | |
H4 | 0.37170 | 0.21660 | 0.23780 | 0.0550* | |
H7 | 0.39030 | 0.17060 | 0.08000 | 0.0520* | |
H8 | 0.40350 | 0.12530 | −0.09080 | 0.0600* | |
H9 | 0.35350 | 0.07350 | −0.18160 | 0.0580* | |
H10 | 0.29250 | 0.06720 | −0.09670 | 0.0480* | |
H11 | 0.22400 | 0.04360 | 0.36910 | 0.0520* | |
H12 | 0.16660 | 0.04370 | 0.47250 | 0.0640* | |
H13 | 0.11240 | 0.09340 | 0.40270 | 0.0740* | |
H14 | 0.11820 | 0.14460 | 0.23290 | 0.0630* | |
H17 | 0.12750 | 0.19010 | 0.07170 | 0.0590* | |
H18 | 0.14270 | 0.23700 | −0.09960 | 0.0650* | |
H19 | 0.20610 | 0.23130 | −0.16990 | 0.0580* | |
H20 | 0.25200 | 0.17670 | −0.07440 | 0.0510* | |
H81 | 0.28390 | −0.01040 | 0.22290 | 0.0600* | |
H82 | 0.30140 | 0.02930 | 0.27360 | 0.0600* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0252 (2) | 0.0302 (2) | 0.0298 (2) | −0.0039 (1) | −0.0005 (2) | −0.0007 (2) |
Cr1 | 0.0261 (2) | 0.0332 (2) | 0.0266 (2) | −0.0036 (2) | −0.0007 (2) | −0.0016 (2) |
Cr2 | 0.0535 (3) | 0.0312 (2) | 0.0425 (3) | 0.0009 (2) | −0.0066 (3) | −0.0028 (3) |
O1 | 0.0386 (12) | 0.0434 (13) | 0.0389 (12) | −0.0137 (10) | −0.0002 (12) | −0.0056 (12) |
O2 | 0.0471 (14) | 0.0634 (18) | 0.0380 (14) | −0.0111 (12) | 0.0122 (13) | −0.0054 (13) |
O3 | 0.0293 (12) | 0.0728 (19) | 0.0359 (13) | −0.0046 (12) | −0.0068 (10) | −0.0028 (13) |
O4 | 0.085 (2) | 0.0444 (16) | 0.0456 (16) | 0.0190 (14) | −0.0013 (17) | 0.0017 (15) |
O5 | 0.109 (3) | 0.0484 (18) | 0.079 (3) | −0.0069 (19) | −0.033 (2) | −0.0191 (19) |
O6 | 0.088 (3) | 0.078 (3) | 0.072 (2) | −0.025 (2) | −0.001 (2) | 0.025 (2) |
O7 | 0.065 (2) | 0.063 (2) | 0.079 (2) | 0.0189 (17) | −0.0118 (18) | −0.020 (2) |
O8 | 0.0637 (18) | 0.0398 (14) | 0.0458 (16) | −0.0027 (13) | −0.0226 (14) | 0.0048 (12) |
N1 | 0.0287 (12) | 0.0322 (14) | 0.0340 (14) | −0.0041 (10) | 0.0004 (11) | −0.0009 (12) |
N2 | 0.0292 (12) | 0.0343 (14) | 0.0345 (13) | −0.0015 (10) | 0.0018 (12) | −0.0001 (12) |
N3 | 0.0328 (13) | 0.0369 (14) | 0.0313 (13) | −0.0077 (12) | 0.0003 (11) | −0.0025 (12) |
N4 | 0.0328 (14) | 0.0316 (14) | 0.0379 (16) | −0.0026 (11) | −0.0009 (12) | 0.0008 (12) |
C1 | 0.0391 (17) | 0.0362 (18) | 0.0387 (17) | −0.0036 (14) | 0.0028 (14) | −0.0053 (16) |
C2 | 0.053 (2) | 0.0390 (18) | 0.042 (2) | −0.0019 (15) | −0.0050 (17) | −0.0076 (16) |
C3 | 0.048 (2) | 0.050 (2) | 0.043 (2) | −0.0158 (17) | −0.0069 (16) | −0.0072 (18) |
C4 | 0.0343 (17) | 0.056 (2) | 0.048 (2) | −0.0175 (16) | −0.0015 (15) | −0.0031 (18) |
C5 | 0.0264 (14) | 0.0342 (16) | 0.0365 (16) | −0.0044 (12) | −0.0002 (12) | 0.0015 (13) |
C6 | 0.0253 (14) | 0.0356 (16) | 0.0384 (17) | −0.0011 (12) | −0.0003 (12) | 0.0036 (14) |
C7 | 0.0286 (15) | 0.053 (2) | 0.048 (2) | −0.0053 (14) | 0.0046 (15) | 0.0029 (19) |
C8 | 0.0353 (18) | 0.065 (3) | 0.051 (2) | 0.0004 (18) | 0.0116 (16) | 0.005 (2) |
C9 | 0.050 (2) | 0.056 (2) | 0.0379 (18) | 0.0054 (16) | 0.0113 (17) | −0.0012 (19) |
C10 | 0.0409 (18) | 0.0447 (19) | 0.0346 (17) | −0.0021 (15) | 0.0023 (14) | −0.0017 (15) |
C11 | 0.048 (2) | 0.046 (2) | 0.0359 (17) | −0.0089 (16) | 0.0019 (15) | −0.0020 (16) |
C12 | 0.067 (3) | 0.052 (2) | 0.041 (2) | −0.012 (2) | 0.019 (2) | −0.0011 (19) |
C13 | 0.059 (3) | 0.064 (3) | 0.063 (3) | −0.004 (2) | 0.034 (2) | −0.009 (2) |
C14 | 0.044 (2) | 0.055 (2) | 0.059 (3) | 0.0080 (18) | 0.0168 (18) | −0.007 (2) |
C15 | 0.0334 (16) | 0.0370 (17) | 0.0391 (18) | −0.0003 (14) | 0.0049 (14) | −0.0078 (15) |
C16 | 0.0314 (15) | 0.0329 (16) | 0.0392 (17) | 0.0023 (12) | 0.0024 (13) | −0.0080 (14) |
C17 | 0.0399 (18) | 0.056 (2) | 0.052 (2) | 0.0160 (16) | 0.0000 (18) | −0.003 (2) |
C18 | 0.058 (2) | 0.049 (2) | 0.054 (2) | 0.021 (2) | −0.011 (2) | −0.002 (2) |
C19 | 0.063 (2) | 0.0373 (18) | 0.044 (2) | 0.0046 (16) | −0.003 (2) | 0.0024 (17) |
C20 | 0.0406 (19) | 0.043 (2) | 0.043 (2) | −0.0020 (15) | 0.0033 (15) | 0.0082 (16) |
Ni1—O1 | 2.083 (2) | C6—C7 | 1.399 (5) |
Ni1—O8 | 2.086 (3) | C7—C8 | 1.365 (6) |
Ni1—N1 | 2.054 (3) | C8—C9 | 1.384 (6) |
Ni1—N2 | 2.081 (3) | C9—C10 | 1.382 (5) |
Ni1—N3 | 2.057 (3) | C11—C12 | 1.381 (6) |
Ni1—N4 | 2.083 (3) | C12—C13 | 1.368 (6) |
Cr1—O1 | 1.629 (3) | C13—C14 | 1.377 (7) |
Cr1—O2 | 1.580 (3) | C14—C15 | 1.383 (5) |
Cr1—O3 | 1.640 (3) | C15—C16 | 1.482 (5) |
Cr1—O4 | 1.744 (3) | C16—C17 | 1.388 (5) |
Cr2—O4 | 1.812 (3) | C17—C18 | 1.394 (6) |
Cr2—O5 | 1.596 (4) | C18—C19 | 1.366 (6) |
Cr2—O6 | 1.589 (4) | C19—C20 | 1.372 (6) |
Cr2—O7 | 1.601 (4) | C1—H1 | 0.9299 |
O8—H81 | 0.9292 | C2—H2 | 0.9288 |
O8—H82 | 0.7734 | C3—H3 | 0.9300 |
N1—C1 | 1.334 (5) | C4—H4 | 0.9315 |
N1—C5 | 1.358 (4) | C7—H7 | 0.9298 |
N2—C10 | 1.339 (5) | C8—H8 | 0.9305 |
N2—C6 | 1.348 (4) | C9—H9 | 0.9294 |
N3—C15 | 1.353 (5) | C10—H10 | 0.9285 |
N3—C11 | 1.332 (5) | C11—H11 | 0.9289 |
N4—C20 | 1.342 (5) | C12—H12 | 0.9305 |
N4—C16 | 1.342 (4) | C13—H13 | 0.9291 |
C1—C2 | 1.390 (5) | C14—H14 | 0.9310 |
C2—C3 | 1.369 (6) | C17—H17 | 0.9297 |
C3—C4 | 1.376 (6) | C18—H18 | 0.9297 |
C4—C5 | 1.391 (5) | C19—H19 | 0.9298 |
C5—C6 | 1.467 (5) | C20—H20 | 0.9300 |
Cr1···C15 | 4.020 (4) | C7···C18viii | 3.510 (6) |
Cr1···C4i | 3.956 (4) | C9···O2iii | 3.351 (6) |
Cr1···C14ii | 3.943 (4) | C10···C12iii | 3.551 (6) |
Cr1···O8iii | 3.770 (4) | C10···O6iii | 3.414 (6) |
Cr2···C20iv | 3.822 (4) | C11···O2 | 3.118 (5) |
Cr2···C19iv | 3.822 (5) | C11···C1 | 3.566 (5) |
Cr2···C1iii | 3.886 (4) | C11···O4iv | 3.331 (5) |
Cr2···C2iii | 3.812 (4) | C12···C10iv | 3.551 (6) |
Cr1···H81 | 3.4747 | C14···C3i | 3.488 (6) |
Cr1···H4i | 3.1446 | C14···Cr1xi | 3.943 (4) |
Cr1···H11iii | 3.2097 | C15···Cr1 | 4.020 (4) |
Cr1···H82iii | 3.1464 | C15···O2 | 3.373 (5) |
Cr1···H14ii | 3.1399 | C17···O3xi | 3.263 (5) |
Cr2···H81 | 3.1236 | C17···C4viii | 3.562 (6) |
Cr2···H1iii | 3.4350 | C18···C7viii | 3.510 (6) |
Cr2···H2iii | 3.3284 | C18···C7i | 3.426 (6) |
Cr2···H19iv | 3.4227 | C19···Cr2iii | 3.822 (5) |
Cr2···H20iv | 3.3933 | C19···C20viii | 3.589 (6) |
Cr2···H8v | 3.2459 | C20···C20viii | 3.579 (5) |
O2···C9iv | 3.351 (6) | C20···O5iii | 3.348 (6) |
O2···N3 | 3.022 (4) | C20···Cr2iii | 3.822 (4) |
O2···C11 | 3.118 (5) | C20···O6iii | 3.394 (6) |
O2···C15 | 3.373 (5) | C20···C19viii | 3.589 (6) |
O2···C3i | 3.285 (5) | C2···H1viii | 3.0942 |
O3···C4i | 3.265 (5) | C4···H7 | 2.7565 |
O3···C17ii | 3.263 (5) | C7···H4 | 2.7543 |
O3···O8iii | 2.688 (4) | C10···H20 | 2.9031 |
O4···C1iii | 3.049 (5) | C11···H1 | 2.8785 |
O4···C11iii | 3.331 (5) | C14···H17 | 2.7289 |
O4···C2iii | 3.345 (5) | C17···H14 | 2.7222 |
O5···O8 | 2.743 (5) | C19···H20viii | 3.0510 |
O5···C20iv | 3.348 (6) | H1···N3 | 2.6687 |
O6···C10iv | 3.414 (6) | H1···C11 | 2.8785 |
O6···C20iv | 3.394 (6) | H1···Cr2iv | 3.4350 |
O7···C2vi | 3.333 (6) | H1···O4iv | 2.7788 |
O8···O3iv | 2.688 (4) | H1···O7iv | 2.8102 |
O8···Cr1iv | 3.770 (4) | H1···C2viii | 3.0942 |
O8···O5 | 2.743 (5) | H2···O7ix | 2.5499 |
O1···H10 | 2.6636 | H2···Cr2iv | 3.3285 |
O2···H3i | 2.6081 | H3···O2x | 2.6081 |
O2···H9iv | 2.5338 | H4···C7 | 2.7543 |
O2···H4i | 2.9121 | H4···H7 | 2.2217 |
O3···H7i | 2.8431 | H4···Cr1x | 3.1446 |
O3···H82iii | 1.9342 | H4···O2x | 2.9121 |
O3···H14ii | 2.5516 | H4···O3x | 2.3681 |
O3···H4i | 2.3681 | H7···C4 | 2.7565 |
O3···H17ii | 2.3794 | H7···H4 | 2.2217 |
O3···H81iii | 2.8161 | H7···O3x | 2.8431 |
O4···H1iii | 2.7788 | H8···Cr2xii | 3.2458 |
O4···H11iii | 2.7654 | H8···O5xii | 2.7777 |
O5···H81 | 1.8154 | H8···O7xii | 2.6038 |
O5···H8v | 2.7777 | H9···O2iii | 2.5338 |
O5···H82 | 2.8885 | H10···O1 | 2.6636 |
O6···H13ii | 2.8557 | H11···O8 | 2.7922 |
O6···H20iv | 2.6786 | H11···Cr1iv | 3.2097 |
O6···H19vii | 2.6780 | H11···O4iv | 2.7654 |
O7···H1iii | 2.8102 | H13···O6xi | 2.8557 |
O7···H8v | 2.6038 | H14···C17 | 2.7222 |
O7···H2vi | 2.5499 | H14···H17 | 2.1822 |
O8···H11 | 2.7922 | H14···Cr1xi | 3.1399 |
N3···O2 | 3.022 (4) | H14···O3xi | 2.5516 |
N2···H20 | 2.7083 | H17···C14 | 2.7289 |
N3···H1 | 2.6687 | H17···H14 | 2.1822 |
C1···C11 | 3.566 (5) | H17···O3xi | 2.3794 |
C1···Cr2iv | 3.886 (4) | H19···O6xiii | 2.6780 |
C1···O4iv | 3.049 (5) | H19···Cr2iii | 3.4227 |
C1···C2viii | 3.492 (5) | H20···N2 | 2.7083 |
C2···O7ix | 3.333 (6) | H20···C10 | 2.9031 |
C2···Cr2iv | 3.812 (4) | H20···Cr2iii | 3.3933 |
C2···O4iv | 3.345 (5) | H20···O6iii | 2.6786 |
C2···C1viii | 3.492 (5) | H20···C19viii | 3.0510 |
C2···C2viii | 3.547 (5) | H81···Cr1 | 3.4747 |
C3···O2x | 3.285 (5) | H81···Cr2 | 3.1236 |
C3···C14x | 3.488 (6) | H81···O5 | 1.8154 |
C4···O3x | 3.265 (5) | H81···O3iv | 2.8161 |
C4···C17viii | 3.562 (6) | H82···O5 | 2.8885 |
C4···Cr1x | 3.956 (4) | H82···Cr1iv | 3.1464 |
C7···C18x | 3.426 (6) | H82···O3iv | 1.9342 |
O1—Ni1—O8 | 82.90 (11) | N2—C6—C5 | 115.7 (3) |
O1—Ni1—N1 | 169.26 (10) | N2—C6—C7 | 120.5 (3) |
O1—Ni1—N2 | 93.42 (11) | C6—C7—C8 | 120.0 (4) |
O1—Ni1—N3 | 92.09 (11) | C7—C8—C9 | 119.0 (4) |
O1—Ni1—N4 | 88.10 (11) | C8—C9—C10 | 119.0 (4) |
O8—Ni1—N1 | 89.08 (12) | N2—C10—C9 | 122.0 (3) |
O8—Ni1—N2 | 87.40 (12) | N3—C11—C12 | 122.9 (4) |
O8—Ni1—N3 | 98.22 (13) | C11—C12—C13 | 118.9 (4) |
O8—Ni1—N4 | 170.57 (12) | C12—C13—C14 | 118.9 (4) |
N1—Ni1—N2 | 79.04 (12) | C13—C14—C15 | 119.7 (4) |
N1—Ni1—N3 | 96.13 (12) | N3—C15—C14 | 121.3 (3) |
N1—Ni1—N4 | 100.20 (12) | N3—C15—C16 | 115.2 (3) |
N2—Ni1—N3 | 172.58 (11) | C14—C15—C16 | 123.6 (3) |
N2—Ni1—N4 | 96.00 (12) | C15—C16—C17 | 123.2 (3) |
N3—Ni1—N4 | 79.21 (12) | N4—C16—C15 | 115.7 (3) |
O1—Cr1—O2 | 111.12 (14) | N4—C16—C17 | 121.1 (3) |
O1—Cr1—O3 | 109.40 (14) | C16—C17—C18 | 118.9 (4) |
O1—Cr1—O4 | 109.72 (15) | C17—C18—C19 | 119.3 (4) |
O2—Cr1—O3 | 109.27 (15) | C18—C19—C20 | 119.0 (4) |
O2—Cr1—O4 | 111.34 (16) | N4—C20—C19 | 122.5 (3) |
O3—Cr1—O4 | 105.85 (16) | N1—C1—H1 | 118.31 |
O4—Cr2—O5 | 108.93 (18) | C2—C1—H1 | 118.28 |
O4—Cr2—O6 | 109.3 (2) | C1—C2—H2 | 121.12 |
O4—Cr2—O7 | 104.9 (2) | C3—C2—H2 | 120.93 |
O5—Cr2—O6 | 111.8 (2) | C2—C3—H3 | 120.12 |
O5—Cr2—O7 | 111.0 (2) | C4—C3—H3 | 120.28 |
O6—Cr2—O7 | 110.7 (2) | C3—C4—H4 | 120.01 |
Ni1—O1—Cr1 | 140.73 (14) | C5—C4—H4 | 119.98 |
Cr1—O4—Cr2 | 129.2 (2) | C6—C7—H7 | 120.10 |
Ni1—O8—H82 | 132.35 | C8—C7—H7 | 119.95 |
H81—O8—H82 | 92.82 | C7—C8—H8 | 120.41 |
Ni1—O8—H81 | 131.75 | C9—C8—H8 | 120.57 |
Ni1—N1—C1 | 126.3 (2) | C8—C9—H9 | 120.50 |
Ni1—N1—C5 | 115.0 (2) | C10—C9—H9 | 120.46 |
C1—N1—C5 | 118.5 (3) | N2—C10—H10 | 119.03 |
C6—N2—C10 | 119.5 (3) | C9—C10—H10 | 118.96 |
Ni1—N2—C6 | 113.9 (2) | N3—C11—H11 | 118.60 |
Ni1—N2—C10 | 126.1 (2) | C12—C11—H11 | 118.47 |
Ni1—N3—C11 | 126.5 (3) | C11—C12—H12 | 120.47 |
Ni1—N3—C15 | 115.2 (3) | C13—C12—H12 | 120.62 |
C11—N3—C15 | 118.3 (3) | C12—C13—H13 | 120.47 |
C16—N4—C20 | 119.1 (3) | C14—C13—H13 | 120.65 |
Ni1—N4—C20 | 126.1 (2) | C13—C14—H14 | 120.22 |
Ni1—N4—C16 | 114.5 (2) | C15—C14—H14 | 120.06 |
N1—C1—C2 | 123.4 (3) | C16—C17—H17 | 120.44 |
C1—C2—C3 | 118.0 (4) | C18—C17—H17 | 120.61 |
C2—C3—C4 | 119.6 (4) | C17—C18—H18 | 120.33 |
C3—C4—C5 | 120.0 (3) | C19—C18—H18 | 120.40 |
N1—C5—C4 | 120.5 (3) | C18—C19—H19 | 120.58 |
N1—C5—C6 | 115.2 (3) | C20—C19—H19 | 120.40 |
C4—C5—C6 | 124.3 (3) | N4—C20—H20 | 118.72 |
C5—C6—C7 | 123.8 (3) | C19—C20—H20 | 118.78 |
O8—Ni1—O1—Cr1 | 79.9 (2) | C1—N1—C5—C6 | 179.4 (3) |
N2—Ni1—O1—Cr1 | 166.9 (2) | Ni1—N1—C5—C6 | 4.1 (4) |
N3—Ni1—O1—Cr1 | −18.1 (2) | Ni1—N2—C6—C5 | −10.7 (4) |
N4—Ni1—O1—Cr1 | −97.2 (2) | Ni1—N2—C6—C7 | 170.0 (3) |
O8—Ni1—N1—C1 | −94.8 (3) | C10—N2—C6—C5 | 177.7 (3) |
O8—Ni1—N1—C5 | 80.1 (3) | C10—N2—C6—C7 | −1.6 (5) |
N2—Ni1—N1—C1 | 177.7 (3) | Ni1—N2—C10—C9 | −168.0 (3) |
N2—Ni1—N1—C5 | −7.4 (2) | C6—N2—C10—C9 | 2.5 (5) |
N3—Ni1—N1—C1 | 3.4 (3) | Ni1—N3—C11—C12 | −179.2 (3) |
N3—Ni1—N1—C5 | 178.3 (3) | Ni1—N3—C15—C14 | 177.8 (3) |
N4—Ni1—N1—C1 | 83.5 (3) | Ni1—N3—C15—C16 | −1.5 (4) |
N4—Ni1—N1—C5 | −101.6 (3) | C11—N3—C15—C14 | −1.7 (5) |
O1—Ni1—N2—C6 | −162.4 (2) | C11—N3—C15—C16 | 178.9 (3) |
O1—Ni1—N2—C10 | 8.5 (3) | C15—N3—C11—C12 | 0.3 (6) |
O8—Ni1—N2—C6 | −79.7 (2) | Ni1—N4—C16—C17 | −174.6 (3) |
O8—Ni1—N2—C10 | 91.2 (3) | C20—N4—C16—C15 | 179.2 (3) |
N1—Ni1—N2—C6 | 9.9 (2) | Ni1—N4—C16—C15 | 4.9 (4) |
N1—Ni1—N2—C10 | −179.2 (3) | C16—N4—C20—C19 | 1.0 (6) |
N4—Ni1—N2—C6 | 109.1 (2) | C20—N4—C16—C17 | −0.4 (5) |
N4—Ni1—N2—C10 | −79.9 (3) | Ni1—N4—C20—C19 | 174.5 (3) |
O1—Ni1—N3—C11 | 95.0 (3) | N1—C1—C2—C3 | −0.3 (6) |
O1—Ni1—N3—C15 | −84.5 (3) | C1—C2—C3—C4 | 0.2 (6) |
O8—Ni1—N3—C11 | 11.8 (3) | C2—C3—C4—C5 | −0.5 (6) |
O8—Ni1—N3—C15 | −167.6 (3) | C3—C4—C5—N1 | 0.9 (6) |
N1—Ni1—N3—C11 | −78.1 (3) | C3—C4—C5—C6 | −179.6 (4) |
N1—Ni1—N3—C15 | 102.4 (3) | N1—C5—C6—N2 | 4.5 (4) |
N4—Ni1—N3—C11 | −177.4 (3) | N1—C5—C6—C7 | −176.2 (3) |
N4—Ni1—N3—C15 | 3.1 (3) | C4—C5—C6—N2 | −175.0 (3) |
O1—Ni1—N4—C16 | 88.1 (3) | C4—C5—C6—C7 | 4.2 (6) |
O1—Ni1—N4—C20 | −85.7 (3) | N2—C6—C7—C8 | −0.5 (6) |
N1—Ni1—N4—C16 | −98.8 (3) | C5—C6—C7—C8 | −179.7 (4) |
N1—Ni1—N4—C20 | 87.4 (3) | C6—C7—C8—C9 | 1.7 (6) |
N2—Ni1—N4—C16 | −178.7 (3) | C7—C8—C9—C10 | −0.8 (6) |
N2—Ni1—N4—C20 | 7.5 (3) | C8—C9—C10—N2 | −1.3 (6) |
N3—Ni1—N4—C16 | −4.4 (2) | N3—C11—C12—C13 | 1.2 (7) |
N3—Ni1—N4—C20 | −178.2 (3) | C11—C12—C13—C14 | −1.3 (7) |
O2—Cr1—O4—Cr2 | −42.0 (3) | C12—C13—C14—C15 | 0.0 (7) |
O3—Cr1—O4—Cr2 | −160.7 (2) | C13—C14—C15—N3 | 1.6 (6) |
O2—Cr1—O1—Ni1 | 7.9 (3) | C13—C14—C15—C16 | −179.1 (4) |
O3—Cr1—O1—Ni1 | 128.6 (2) | N3—C15—C16—N4 | −2.3 (5) |
O4—Cr1—O1—Ni1 | −115.7 (2) | N3—C15—C16—C17 | 177.3 (4) |
O1—Cr1—O4—Cr2 | 81.4 (3) | C14—C15—C16—C17 | −2.1 (6) |
O6—Cr2—O4—Cr1 | 83.0 (3) | C14—C15—C16—N4 | 178.3 (4) |
O7—Cr2—O4—Cr1 | −158.3 (3) | N4—C16—C17—C18 | 0.2 (6) |
O5—Cr2—O4—Cr1 | −39.4 (3) | C15—C16—C17—C18 | −179.3 (4) |
C5—N1—C1—C2 | 0.8 (5) | C16—C17—C18—C19 | −0.6 (6) |
Ni1—N1—C5—C4 | −176.4 (3) | C17—C18—C19—C20 | 1.2 (6) |
Ni1—N1—C1—C2 | 175.5 (3) | C18—C19—C20—N4 | −1.5 (6) |
C1—N1—C5—C4 | −1.1 (5) |
Symmetry codes: (i) x−1/4, −y+1/4, z−1/4; (ii) −x+1/4, y−1/4, z−1/4; (iii) −x+1/2, −y, z−1/2; (iv) −x+1/2, −y, z+1/2; (v) −x+3/4, y−1/4, z+1/4; (vi) x, y−1/2, z−1/2; (vii) x, y−1/2, z+1/2; (viii) −x+1/2, −y+1/2, z; (ix) x, y+1/2, z+1/2; (x) x+1/4, −y+1/4, z+1/4; (xi) −x+1/4, y+1/4, z+1/4; (xii) −x+3/4, y+1/4, z−1/4; (xiii) x, y+1/2, z−1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H81···O5 | 0.929 | 1.815 | 2.743 (5) | 175.30 |
O8—H82···O3iv | 0.773 | 1.934 | 2.688 (4) | 164.83 |
C2—H2···O7ix | 0.929 | 2.550 | 3.333 (6) | 142.27 |
C4—H4···O3x | 0.932 | 2.368 | 3.265 (5) | 161.66 |
C9—H9···O2iii | 0.929 | 2.534 | 3.351 (6) | 146.97 |
C14—H14···O3xi | 0.931 | 2.552 | 3.446 (5) | 161.19 |
C17—H17···O3xi | 0.930 | 2.379 | 3.263 (5) | 158.75 |
Symmetry codes: (iii) −x+1/2, −y, z−1/2; (iv) −x+1/2, −y, z+1/2; (ix) x, y+1/2, z+1/2; (x) x+1/4, −y+1/4, z+1/4; (xi) −x+1/4, y+1/4, z+1/4. |
Experimental details
Crystal data | |
Chemical formula | [NiCr2O7(C10H8N2)2(H2O)] |
Mr | 605.07 |
Crystal system, space group | Orthorhombic, Fdd2 |
Temperature (K) | 293 |
a, b, c (Å) | 33.958 (5), 22.880 (3), 11.735 (1) |
V (Å3) | 9118 (2) |
Z | 16 |
Radiation type | Mo Kα |
µ (mm−1) | 1.81 |
Crystal size (mm) | 0.45 × 0.23 × 0.15 |
Data collection | |
Diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.613, 0.762 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3459, 3459, 2927 |
Rint | 0.000 |
(sin θ/λ)max (Å−1) | 0.703 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.029, 0.075, 1.08 |
No. of reflections | 3459 |
No. of parameters | 316 |
No. of restraints | 1 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.47, −0.28 |
Absolute structure | (Flack, 1983). No Fridel pairs. |
Absolute structure parameter | 0.07 (2) |
Computer programs: CAD-4 EXPRESS (Enraf-Nonius, 1994), CAD-4 EXPRESS, HELENA (Spek, 1997), SIR97 (Altomare et al., 1998), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 1990), PLATON.
Ni1—O1 | 2.083 (2) | Cr1—O2 | 1.580 (3) |
Ni1—O8 | 2.086 (3) | Cr1—O3 | 1.640 (3) |
Ni1—N1 | 2.054 (3) | Cr1—O4 | 1.744 (3) |
Ni1—N2 | 2.081 (3) | Cr2—O4 | 1.812 (3) |
Ni1—N3 | 2.057 (3) | Cr2—O5 | 1.596 (4) |
Ni1—N4 | 2.083 (3) | Cr2—O6 | 1.589 (4) |
Cr1—O1 | 1.629 (3) | Cr2—O7 | 1.601 (4) |
O1—Ni1—N1 | 169.26 (10) | Ni1—O1—Cr1 | 140.73 (14) |
O8—Ni1—N4 | 170.57 (12) | Cr1—O4—Cr2 | 129.2 (2) |
N2—Ni1—N3 | 172.58 (11) |
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H81···O5 | 0.929 | 1.815 | 2.743 (5) | 175.30 |
O8—H82···O3i | 0.773 | 1.934 | 2.688 (4) | 164.83 |
Symmetry code: (i) −x+1/2, −y, z+1/2. |
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The industrial importance of chromium(VI) compounds, together with their toxic and genotoxic character, are the reasons for considerable attention attracted by the studies of the metal complexes containing compounds of chromium(VI) as ligands (Dave & Czernuszewiccz, 1994). In particular, a coordination model based on the study of chromates and dichromate complexes of transition metals with organic ligands, has been proposed to explain the decrease in the mutagenic activities of the chromium(VI) compounds (Gili & Lorenzo-Luis, 1999).
Many transition metal complexes containing [Cr2O7]2- and organic bases as ligands have been structurally characterized (Uggla et al., 1970; Jameson et al., 1986; Munno et al., 1998; Pan et al., 1998) because of their special properties in such areas as analytical chemistry, catalysis and magneto-chemistry.
In our current research on dichromate complexes of transition metals with magnetic properties, we have prepared a new nickel(II) dichromate with bipy as chelating ligand (Fig. 1). The asymmetric unit of the title complex, (I), involves an NiII atom with a distorted octahedral coordination environment provided by a pair of chelating bipy ligands, water molecule and O atom of the Cr2O7 group, oxygen ligands occupying cis positions in the octahedron. The Ni—Nbipy bond distances [mean value 2.068 (3) Å] are slightly shorter than the Ni—Owater bond length [2.086 (3) Å]. The N—Ni—N bite angles [79.04 (12) and 79.21 (12)°] agree well with those reported previously for other nickel(II) complexes containing bipy (Wada et al., 1976; Cortés et al., 1994; Román et al., 1995; Hernández-Molina et al., 1999). As expected, both bipy ligands are nearly planar [the largest deviation from their mean planes is 0.069 (4) Å for C10], the certain degree of twisting of the pyridyl rings in the bipy ligands relative to each other [in the title compound, the twist angles are 5.1 (2) and 2.1 (2)° for N1/N2/C1–C10 and N3/N4/C11–C20, respectively] is perfectly normal; angles up to 18° have been observed previously (Cano et al., 1994). The mean planes of the two bipy molecules are inclined by 71.67 (10)° with respect to one another.
Each Cr atom in (I) exhibits a slightly distorted tetahedral geometry. The two tetahedral CrO4 groups share one O atom (O4) thus forming a dichromate anion in an almost eclipsed conformation. The Cr—O—Cr bridging angle is 129.2 (2)°, a value which is in the range of previously reported dichromate-containing compounds (Mestres et al., 1993; Martín-Zarza et al., 1995). The bridging Cr—O bonds are 1.744 (3) and 1.812 (3) Å for Cr1—O4 and Cr2—O4, respectively. They are longer than the terminal Cr—O bonds, the maximum and minimum bond lengths for the latter being 1.640 (3) (Cr1—O3) and 1.580 (3) Å (Cr1—O2). The O—Cr—O bond angle range is 104.9 (2)–111.8 (2)° and Cr—O—Ni bridging angle [140.73 (14)°] is in accordance with the analogous parameters in similar compounds (Oshio et al., 1997; Ki-Young et al., 1999).
The water molecule coordinated to the NiII atom forms one intramolecular hydrogen bond with the terminal O atom of the dichromate ligand [O8···O5 2.743 (5) Å], as well as one intermolecular hydrogen bond [O8···O3i 2.688 (4) Å; symmetry code: (i) 1/2 - x, -y, 1/2 + z] (Fig. 2). The latter hydrogen bond links the molecules of the complex into the infinite chains stretching along the c axis of the crystal.