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The title compound, [Ni2(C2O4)(C4H13N3)2(H2O)2][B(C6H5)4]2, contains a centrosymmetric dinuclear oxalato–nickel(II) complex cation in which the oxalate ligand bridges the Ni atoms in a bis-bidentate fashion. The distorted octahedral environment of each Ni atom is completed by the three N atoms of the diethyl­enetri­amine ligand in a fac arrangement, and by one O atom from a water mol­ecule. Tetra­phenyl­borate acts as the counter-anion. The crystal structure shows alternate cationic and anionic layers packed along the [10\overline 1] direction.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803016362/fl6050sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803016362/fl6050Isup2.hkl
Contains datablock I

CCDC reference: 221662

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.045
  • wR factor = 0.125
  • Data-to-parameter ratio = 23.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
PLAT_420 Alert B D-H Without Acceptor O3 - H31W ... ? PLAT_420 Alert B D-H Without Acceptor O3 - H32W ... ?
Yellow Alert Alert Level C:
PLAT_369 Alert C Long C(sp2)-C(sp2) Bond C1 - C1_a = 1.56 Ang. PLAT_420 Alert C D-H Without Acceptor N1 - H1A ... ? PLAT_420 Alert C D-H Without Acceptor N1 - H1B ... ? PLAT_420 Alert C D-H Without Acceptor N4 - H4 ... ? PLAT_420 Alert C D-H Without Acceptor N7 - H7A ... ? PLAT_420 Alert C D-H Without Acceptor N7 - H7B ... ?
0 Alert Level A = Potentially serious problem
2 Alert Level B = Potential problem
6 Alert Level C = Please check

Computing details top

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994); cell refinement: CAD-4 EXPRESS (Enraf-Nonius, 1994); data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: DIRDIF99.2 (Beurskens et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 2002); software used to prepare material for publication: WinGX (Farrugia, 1999).

(I) top
Crystal data top
[Ni2(C2O4)(C4H13N3)2(H2O)2](C24H20B)2F(000) = 1148
Mr = 1086.24Dx = 1.319 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 25 reflections
a = 10.850 (1) Åθ = 9.6–12.3°
b = 19.576 (3) ŵ = 0.74 mm1
c = 13.020 (2) ÅT = 293 K
β = 98.52 (1)°Prism, blue
V = 2734.9 (6) Å30.5 × 0.3 × 0.25 mm
Z = 2
Data collection top
Enraf-Nonius CAD-4
diffractometer
θmax = 30.0°, θmin = 1.9°
Radiation source: x-ray tubeh = 1515
ω/2θ scansk = 027
8287 measured reflectionsl = 018
7975 independent reflections2 standard reflections every 100 reflections
4921 reflections with I > 2σ(I) intensity decay: 4%
Rint = 0.046
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.045 w = 1/[σ2(Fo2) + (0.057P)2 + 0.7675P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.126(Δ/σ)max = 0.001
S = 1.01Δρmax = 0.43 e Å3
7975 reflectionsΔρmin = 0.50 e Å3
343 parameters
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.10145 (2)0.083678 (15)0.15272 (2)0.04100 (9)
O10.03939 (14)0.08394 (8)0.02725 (13)0.0477 (4)
O20.13374 (13)0.01074 (9)0.09089 (13)0.0470 (4)
O30.01293 (19)0.03830 (12)0.24975 (19)0.0645 (6)
H31W0.001 (3)0.0004 (19)0.259 (3)0.077*
H32W0.081 (3)0.0488 (18)0.249 (3)0.077*
N70.04478 (19)0.18027 (11)0.19259 (18)0.0539 (5)
H7A0.0236 (15)0.1886 (2)0.1606 (7)0.065*
H7B0.0398 (2)0.18134 (11)0.2541 (14)0.065*
C310.31000 (18)0.02785 (11)0.75333 (18)0.0383 (5)
N40.22828 (17)0.13878 (11)0.07978 (17)0.0478 (5)
H40.22892 (17)0.1221 (6)0.017 (2)0.057*
N10.25872 (19)0.06484 (13)0.26221 (18)0.0568 (6)
H1A0.2670 (3)0.0959 (7)0.3105 (11)0.068*
H1B0.2539 (2)0.0249 (9)0.2908 (7)0.068*
C260.4926 (2)0.14406 (13)0.84034 (19)0.0480 (6)
H260.52770.10390.81980.058*
C350.2937 (2)0.09439 (12)0.7182 (2)0.0541 (6)
H350.2830.12960.66970.065*
C110.1406 (2)0.11687 (11)0.69189 (18)0.0410 (5)
C330.3272 (3)0.05662 (15)0.8925 (2)0.0590 (7)
H330.33860.06590.96330.071*
C210.36811 (19)0.15858 (11)0.80057 (16)0.0373 (4)
C10.05030 (19)0.02752 (12)0.01816 (18)0.0413 (5)
C320.3277 (2)0.01021 (13)0.85867 (19)0.0470 (5)
H320.34020.04490.90790.056*
C160.0685 (2)0.13391 (14)0.7686 (2)0.0542 (6)
H160.10880.1460.83420.065*
C430.3778 (3)0.20691 (16)0.4717 (2)0.0594 (7)
H430.35310.24760.43790.071*
C450.5053 (3)0.10830 (15)0.4904 (2)0.0612 (7)
H450.56810.08180.46920.073*
C440.4693 (3)0.16752 (17)0.4388 (2)0.0617 (7)
H440.50630.1810.3820.074*
C360.2928 (2)0.02693 (12)0.6851 (2)0.0454 (5)
H360.28020.01810.61410.055*
C120.0731 (2)0.09787 (13)0.5963 (2)0.0538 (6)
H120.11660.08610.54250.065*
C30.3543 (2)0.13224 (16)0.1401 (2)0.0610 (7)
H3A0.37110.1710.18650.073*
H3B0.4160.13210.09320.073*
B10.2931 (2)0.10752 (13)0.71432 (19)0.0363 (5)
C340.3103 (2)0.10924 (14)0.8226 (3)0.0595 (7)
H340.310.15430.84530.071*
C130.0562 (3)0.09590 (16)0.5785 (3)0.0721 (10)
H130.09750.08190.51420.086*
C20.3639 (2)0.06730 (15)0.2019 (2)0.0581 (7)
H2A0.36060.02820.15580.07*
H2B0.44240.0660.24850.07*
C140.1235 (3)0.11465 (18)0.6559 (3)0.0807 (11)
H140.21010.11450.64370.097*
C220.3239 (2)0.22067 (12)0.83299 (19)0.0456 (5)
H220.2430.23390.80710.055*
C410.3548 (2)0.12486 (12)0.60957 (17)0.0394 (5)
C240.5162 (3)0.24677 (15)0.9406 (2)0.0605 (7)
H240.56430.27550.98740.073*
C460.4486 (2)0.08734 (13)0.5744 (2)0.0506 (6)
H460.47470.04680.60810.061*
C60.1342 (3)0.23198 (14)0.1686 (2)0.0564 (6)
H6A0.20250.23570.22540.068*
H6B0.09370.27620.15840.068*
C50.1824 (3)0.21014 (15)0.0708 (2)0.0587 (7)
H5A0.11610.21380.01220.07*
H5B0.24960.24020.05830.07*
C420.3229 (2)0.18560 (14)0.55553 (19)0.0495 (6)
H420.26160.21310.5770.059*
C150.0614 (3)0.13354 (17)0.7509 (3)0.0723 (9)
H150.10590.14620.80360.087*
C230.3965 (3)0.26354 (14)0.9027 (2)0.0577 (7)
H230.36280.3040.92350.069*
C250.5655 (2)0.18710 (15)0.9091 (2)0.0576 (7)
H250.64770.17550.93380.069*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.03954 (13)0.04095 (16)0.04260 (18)0.00240 (12)0.00636 (11)0.00702 (14)
O10.0478 (8)0.0398 (9)0.0530 (10)0.0028 (7)0.0004 (7)0.0109 (8)
O20.0433 (7)0.0463 (9)0.0485 (10)0.0023 (7)0.0026 (7)0.0075 (8)
O30.0550 (10)0.0603 (13)0.0826 (15)0.0015 (10)0.0243 (10)0.0123 (12)
N70.0562 (11)0.0547 (13)0.0536 (13)0.0028 (10)0.0179 (10)0.0128 (11)
C310.0384 (9)0.0377 (11)0.0399 (12)0.0018 (8)0.0092 (9)0.0031 (9)
N40.0488 (10)0.0536 (12)0.0422 (12)0.0020 (9)0.0111 (9)0.0026 (10)
N10.0553 (11)0.0663 (15)0.0470 (13)0.0081 (10)0.0011 (10)0.0011 (11)
C260.0518 (12)0.0473 (14)0.0439 (14)0.0005 (10)0.0038 (10)0.0029 (11)
C350.0534 (12)0.0366 (14)0.0730 (19)0.0062 (10)0.0122 (12)0.0054 (12)
C110.0470 (10)0.0344 (11)0.0413 (13)0.0002 (9)0.0054 (9)0.0092 (10)
C330.0677 (15)0.0561 (16)0.0565 (17)0.0098 (13)0.0197 (13)0.0211 (14)
C210.0471 (10)0.0378 (11)0.0272 (11)0.0005 (9)0.0062 (8)0.0039 (9)
C10.0406 (10)0.0413 (12)0.0423 (13)0.0009 (9)0.0068 (9)0.0015 (10)
C320.0594 (13)0.0454 (14)0.0383 (13)0.0062 (10)0.0135 (10)0.0080 (11)
C160.0529 (12)0.0529 (15)0.0589 (17)0.0033 (11)0.0150 (12)0.0032 (13)
C430.0683 (15)0.0687 (18)0.0395 (14)0.0110 (14)0.0025 (12)0.0159 (13)
C450.0786 (17)0.0580 (17)0.0541 (17)0.0065 (14)0.0334 (14)0.0146 (14)
C440.0804 (18)0.074 (2)0.0339 (14)0.0230 (15)0.0194 (13)0.0060 (13)
C360.0482 (11)0.0422 (13)0.0460 (14)0.0044 (9)0.0072 (10)0.0004 (11)
C120.0565 (13)0.0550 (16)0.0464 (15)0.0064 (11)0.0042 (11)0.0151 (12)
C30.0437 (11)0.0703 (19)0.0693 (19)0.0062 (12)0.0097 (12)0.0017 (15)
B10.0449 (11)0.0346 (12)0.0296 (13)0.0004 (9)0.0059 (9)0.0016 (10)
C340.0577 (13)0.0389 (13)0.084 (2)0.0005 (11)0.0188 (14)0.0194 (14)
C130.0607 (15)0.070 (2)0.075 (2)0.0136 (14)0.0227 (15)0.0317 (16)
C20.0408 (11)0.0679 (18)0.0632 (18)0.0025 (11)0.0001 (11)0.0056 (14)
C140.0440 (13)0.075 (2)0.119 (3)0.0002 (14)0.0009 (17)0.041 (2)
C220.0559 (12)0.0405 (13)0.0394 (13)0.0003 (10)0.0038 (10)0.0014 (10)
C410.0469 (10)0.0400 (12)0.0311 (11)0.0054 (9)0.0048 (9)0.0026 (9)
C240.0815 (17)0.0518 (16)0.0417 (15)0.0176 (14)0.0122 (13)0.0003 (12)
C460.0661 (14)0.0424 (13)0.0471 (14)0.0021 (11)0.0203 (11)0.0026 (11)
C60.0729 (16)0.0444 (14)0.0547 (17)0.0017 (12)0.0183 (13)0.0080 (12)
C50.0704 (15)0.0549 (16)0.0543 (17)0.0023 (13)0.0211 (13)0.0033 (13)
C420.0525 (12)0.0528 (15)0.0427 (14)0.0006 (10)0.0057 (10)0.0087 (11)
C150.0540 (14)0.0649 (19)0.103 (3)0.0075 (13)0.0280 (17)0.0147 (18)
C230.0825 (17)0.0432 (14)0.0461 (16)0.0029 (12)0.0053 (13)0.0066 (12)
C250.0551 (13)0.0599 (17)0.0523 (16)0.0110 (12)0.0101 (12)0.0129 (13)
Geometric parameters (Å, º) top
Ni1—O12.065 (2)C16—H160.93
Ni1—O22.067 (2)C43—C441.375 (4)
Ni1—O32.095 (2)C43—C421.383 (4)
Ni1—N12.088 (2)C43—H430.93
Ni1—N42.085 (2)C45—C441.367 (4)
Ni1—N72.078 (2)C45—C461.394 (4)
O1—C11.250 (3)C45—H450.93
O2—C1i1.253 (3)C44—H440.93
O3—H31W0.78 (4)C36—H360.93
O3—H32W0.76 (3)C12—C131.388 (4)
N7—C61.467 (3)C12—H120.93
N7—H7A0.8115C3—C21.500 (4)
N7—H7B0.8115C3—H3A0.97
C31—C361.388 (3)C3—H3B0.97
C31—C321.400 (3)B1—C411.641 (3)
N4—C31.478 (3)C34—H340.93
N4—C51.482 (3)C13—C141.379 (5)
N4—H40.8789C13—H130.93
N1—C21.478 (3)C2—H2A0.97
N1—H1A0.8702C2—H2B0.97
N1—H1B0.8702C14—C151.368 (5)
C26—C251.389 (3)C14—H140.93
C26—C211.402 (3)C22—C231.391 (3)
C26—H260.93C22—H220.93
C35—C341.376 (4)C41—C461.387 (3)
C35—C361.389 (3)C41—C421.399 (3)
C35—H350.93C24—C231.360 (4)
C11—C161.397 (3)C24—C251.372 (4)
C11—C121.397 (3)C24—H240.93
B1—C111.647 (3)C46—H460.93
B1—C211.629 (3)C6—C51.508 (4)
B1—C311.642 (3)C6—H6A0.97
C33—C341.369 (4)C6—H6B0.97
C33—C321.381 (4)C5—H5A0.97
C33—H330.93C5—H5B0.97
C21—C221.395 (3)C42—H420.93
C1—O2i1.253 (3)C15—H150.93
C1—C1i1.557 (4)C23—H230.93
C32—H320.93C25—H250.93
C16—C151.394 (4)
O1—Ni1—O280.93 (6)C45—C44—H44120.4
O1—Ni1—N789.07 (8)C43—C44—H44120.4
O2—Ni1—N7169.98 (8)C31—C36—C35122.8 (2)
O1—Ni1—N495.71 (8)C31—C36—H36118.6
O2—Ni1—N497.12 (8)C35—C36—H36118.6
N7—Ni1—N483.26 (8)C13—C12—C11122.6 (3)
O1—Ni1—N1167.10 (8)C13—C12—H12118.7
O2—Ni1—N186.53 (8)C11—C12—H12118.7
N7—Ni1—N1103.43 (9)N4—C3—C2110.1 (2)
N4—Ni1—N182.80 (9)N4—C3—H3A109.6
O1—Ni1—O392.47 (8)C2—C3—H3A109.6
O2—Ni1—O390.31 (8)N4—C3—H3B109.6
N7—Ni1—O390.66 (9)C2—C3—H3B109.6
N1—Ni1—O390.61 (9)H3A—C3—H3B108.2
N4—Ni1—O3169.72 (9)C21—B1—C41102.84 (17)
C1—O1—Ni1112.28 (14)C21—B1—C31110.37 (18)
C1i—O2—Ni1112.55 (14)C21—B1—C11116.13 (19)
Ni1—O3—H31W113 (3)C31—B1—C11102.93 (17)
Ni1—O3—H32W122 (3)C41—B1—C31114.38 (18)
H31W—O3—H32W116 (4)C41—B1—C11110.63 (18)
C6—N7—Ni1110.19 (15)C33—C34—C35118.9 (2)
C6—N7—H7A109.6C33—C34—H34120.6
Ni1—N7—H7A109.6C35—C34—H34120.6
C6—N7—H7B109.6C14—C13—C12120.1 (3)
Ni1—N7—H7B109.6C14—C13—H13119.9
H7A—N7—H7B108.1C12—C13—H13119.9
C36—C31—C32115.0 (2)N1—C2—C3108.4 (2)
C36—C31—B1122.5 (2)N1—C2—H2A110
C32—C31—B1122.0 (2)C3—C2—H2A110
C3—N4—C5113.4 (2)N1—C2—H2B110
C3—N4—Ni1109.55 (16)C3—C2—H2B110
C5—N4—Ni1106.66 (15)H2A—C2—H2B108.4
C3—N4—H4109C15—C14—C13119.3 (3)
C5—N4—H4109C15—C14—H14120.4
Ni1—N4—H4109C13—C14—H14120.4
C2—N1—Ni1104.41 (16)C23—C22—C21122.4 (2)
C2—N1—H1A110.9C23—C22—H22118.8
Ni1—N1—H1A110.9C21—C22—H22118.8
C2—N1—H1B110.9C46—C41—C42115.0 (2)
Ni1—N1—H1B110.9C46—C41—B1125.1 (2)
H1A—N1—H1B108.9C42—C41—B1119.5 (2)
C25—C26—C21122.8 (2)C23—C24—C25119.4 (2)
C25—C26—H26118.6C23—C24—H24120.3
C21—C26—H26118.6C25—C24—H24120.3
C34—C35—C36120.1 (3)C41—C46—C45122.3 (3)
C34—C35—H35119.9C41—C46—H46118.9
C36—C35—H35119.9C45—C46—H46118.9
C16—C11—C12115.2 (2)N7—C6—C5107.9 (2)
C16—C11—B1123.6 (2)N7—C6—H6A110.1
C12—C11—B1120.5 (2)C5—C6—H6A110.1
C34—C33—C32120.5 (3)N7—C6—H6B110.1
C34—C33—H33119.8C5—C6—H6B110.1
C32—C33—H33119.8H6A—C6—H6B108.4
C22—C21—C26114.9 (2)N4—C5—C6110.8 (2)
C22—C21—B1125.76 (19)N4—C5—H5A109.5
C26—C21—B1119.1 (2)C6—C5—H5A109.5
O1—C1—O2i126.6 (2)N4—C5—H5B109.5
O1—C1—C1i117.1 (2)C6—C5—H5B109.5
O2i—C1—C1i116.3 (3)H5A—C5—H5B108.1
C33—C32—C31122.7 (3)C43—C42—C41123.4 (3)
C33—C32—H32118.7C43—C42—H42118.3
C31—C32—H32118.7C41—C42—H42118.3
C15—C16—C11122.6 (3)C14—C15—C16120.1 (3)
C15—C16—H16118.7C14—C15—H15119.9
C11—C16—H16118.7C16—C15—H15119.9
C44—C43—C42119.5 (3)C24—C23—C22120.6 (3)
C44—C43—H43120.2C24—C23—H23119.7
C42—C43—H43120.2C22—C23—H23119.7
C44—C45—C46120.5 (3)C24—C25—C26119.9 (2)
C44—C45—H45119.7C24—C25—H25120
C46—C45—H45119.7C26—C25—H25120
C45—C44—C43119.3 (2)
Symmetry code: (i) x, y, z.
Geometrical parameters (Å,°) of the O—H···π interactions. top
O—H···πO—HH···πO···πO—H···π
O3—H31w···Cg(1)a0.78 (4)2.42 (4)3.168 (3)161 (3)
O3—H32w···Cg(3)b0.76 (3)2.47 (3)3.192 (2)158 (4)
Notes: (a) Cg1 is the centroid of phenyl ring C11i–C16i; (b) Cg3 is the centroid of phenyl ring C31i–C36i.

Symmetry code: (i) -x, -y, 1-z.
 

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