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The title complex, (C25H21NO2P)2[Ni(C4N2S2)2]·2H2O or (NO2BzTPP)2 [Ni(mnt)2]·2H2O [where NO2BzTPP is (4-nitro­benz­yl)tripenylphosphinium and mnt is maleonitrile­dithiol­ate], is reported. The Ni atom lies on a centre of symmetry. The square-planar NiII ion of the anion is coordinated by four S atoms of the two mnt2− ligands. The benzene rings in the [NO2BzTPP]+ cation are twisted with respect to the plane of the P—C—C chain. Weak C—H...Ni inter­actions between the anion and cation and C—H...π, π–π and C—H...O inter­actions between cations are observed in the crystal structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806034386/hg2084sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806034386/hg2084Isup2.hkl
Contains datablock I

CCDC reference: 624715

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.053
  • wR factor = 0.127
  • Data-to-parameter ratio = 14.0

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N3 PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C1 - C2 ... 1.43 Ang. PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C3 - C4 ... 1.43 Ang.
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Bis[(4-nitrobenzyl)tripenylphosphinium] bis(maleonitriledithiolato)nickel(II) dihydrate top
Crystal data top
(C25H21NO2P)2[Ni(C4N2S2)2]·2H2OZ = 1
Mr = 1171.90F(000) = 606
Triclinic, P1Dx = 1.375 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.931 (3) ÅCell parameters from 854 reflections
b = 10.962 (3) Åθ = 2.7–27.8°
c = 12.044 (3) ŵ = 0.60 mm1
α = 82.940 (1)°T = 293 K
β = 82.700 (1)°Block, red
γ = 84.420 (1)°0.45 × 0.32 × 0.18 mm
V = 1415.7 (7) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
4871 independent reflections
Radiation source: fine-focus sealed tube4220 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
φ and ω scansθmax = 25.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1212
Tmin = 0.801, Tmax = 0.897k = 1312
7009 measured reflectionsl = 1314
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.053Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.127H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.056P)2 + 1.5P]
where P = (Fo2 + 2Fc2)/3
4871 reflections(Δ/σ)max < 0.001
349 parametersΔρmax = 0.76 e Å3
0 restraintsΔρmin = 0.87 e Å3
Special details top

Experimental. IR data (KBr, cm-1): 3450 (s), 3060 (w), 2937 (w), 2887 (w), 2190(s), 1602 (s), 1525 (s), 1483 (s), 1438 (s), 1347 (s), 1185 (s), 1147 (s), 1110(m), 996 (m), 861 (m), 774 (m), 744 (m), 721 (m), 688 (m), 634 (m), 530 (s), 506 (s), 453 (m).

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
xyzUiso*/Ueq
Ni10.00000.50001.00000.04386 (17)
S10.00062 (9)0.34164 (8)0.90838 (8)0.0580 (2)
S20.17872 (8)0.54359 (8)0.91436 (8)0.0529 (2)
N10.1925 (4)0.1680 (4)0.6942 (4)0.0930 (12)
N20.4402 (3)0.4257 (3)0.7248 (3)0.0756 (10)
N30.3857 (4)0.8895 (3)1.1502 (3)0.0849 (11)
O10.4401 (4)0.9560 (4)1.1938 (4)0.1323 (16)
O20.2777 (5)0.8764 (5)1.1736 (4)0.158 (2)
O30.0940 (18)0.9932 (12)0.0216 (17)0.49 (2)
H3A0.08630.93780.03410.739*
H3B0.13371.05010.00500.739*
P10.70425 (7)0.64658 (6)0.69410 (6)0.03400 (19)
C10.1716 (4)0.2435 (4)0.7528 (3)0.0625 (9)
C20.1413 (3)0.3392 (3)0.8251 (3)0.0511 (8)
C30.2199 (3)0.4259 (3)0.8289 (3)0.0486 (8)
C40.3413 (4)0.4247 (3)0.7681 (3)0.0568 (9)
C50.6492 (3)0.7503 (3)0.9672 (3)0.0486 (7)
H50.73450.75360.95170.058*
C60.5817 (4)0.8238 (3)1.0432 (3)0.0577 (9)
H60.62080.87691.07910.069*
C70.4567 (4)0.8169 (3)1.0644 (3)0.0555 (9)
C80.3954 (4)0.7419 (3)1.0124 (3)0.0636 (10)
H80.31000.73951.02780.076*
C90.4632 (3)0.6698 (3)0.9364 (3)0.0566 (9)
H90.42280.61890.89930.068*
C100.5895 (3)0.6720 (3)0.9146 (2)0.0407 (7)
C110.6609 (3)0.5836 (3)0.8381 (2)0.0412 (7)
H11A0.61140.51510.83720.049*
H11B0.73570.55080.87060.049*
C120.5136 (3)0.8260 (3)0.6704 (3)0.0574 (9)
H120.54330.85930.72820.069*
C130.4112 (4)0.8823 (4)0.6240 (4)0.0758 (12)
H130.37170.95410.65020.091*
C140.3671 (4)0.8332 (4)0.5396 (4)0.0832 (14)
H140.29760.87160.50860.100*
C150.4249 (4)0.7275 (4)0.5003 (4)0.0720 (11)
H150.39480.69500.44240.086*
C160.5267 (3)0.6696 (3)0.5458 (3)0.0494 (8)
H160.56480.59720.51980.059*
C170.5727 (3)0.7191 (3)0.6307 (3)0.0396 (6)
C180.8030 (3)0.4062 (3)0.6773 (3)0.0470 (7)
H180.77780.39110.75400.056*
C190.8666 (3)0.3136 (3)0.6190 (3)0.0555 (9)
H190.88590.23680.65760.067*
C200.9010 (3)0.3336 (3)0.5065 (3)0.0545 (8)
H200.94260.27020.46840.065*
C210.8746 (3)0.4476 (3)0.4485 (3)0.0543 (8)
H210.89740.46090.37120.065*
C220.8140 (3)0.5422 (3)0.5056 (3)0.0460 (7)
H220.79800.61980.46710.055*
C230.7772 (3)0.5215 (2)0.6199 (2)0.0362 (6)
C240.8102 (3)0.8676 (3)0.6229 (3)0.0506 (8)
H240.74750.88690.57660.061*
C250.8994 (3)0.9486 (3)0.6232 (3)0.0595 (9)
H250.89531.02350.57770.071*
C260.9929 (3)0.9209 (3)0.6887 (3)0.0592 (9)
H261.05170.97680.68830.071*
C271.0005 (3)0.8099 (3)0.7557 (3)0.0563 (8)
H271.06540.79020.79950.068*
C280.9118 (3)0.7281 (3)0.7579 (3)0.0454 (7)
H280.91660.65320.80330.055*
C290.8156 (3)0.7576 (2)0.6923 (2)0.0361 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0447 (3)0.0377 (3)0.0500 (3)0.0100 (2)0.0141 (2)0.0056 (2)
S10.0605 (5)0.0523 (5)0.0645 (6)0.0229 (4)0.0068 (4)0.0061 (4)
S20.0477 (5)0.0445 (5)0.0682 (6)0.0137 (4)0.0081 (4)0.0037 (4)
N10.111 (3)0.074 (3)0.099 (3)0.027 (2)0.005 (2)0.030 (2)
N20.075 (2)0.075 (2)0.076 (2)0.0212 (19)0.0121 (19)0.0127 (18)
N30.110 (3)0.060 (2)0.081 (2)0.006 (2)0.025 (2)0.0294 (19)
O10.158 (4)0.113 (3)0.137 (3)0.017 (3)0.018 (3)0.090 (3)
O20.121 (3)0.174 (5)0.181 (5)0.018 (3)0.068 (3)0.114 (4)
O31.15 (6)0.092 (4)0.333 (16)0.11 (2)0.46 (4)0.047 (7)
P10.0381 (4)0.0261 (3)0.0374 (4)0.0001 (3)0.0045 (3)0.0037 (3)
C10.072 (2)0.055 (2)0.061 (2)0.0205 (19)0.0060 (18)0.0002 (18)
C20.060 (2)0.0471 (18)0.0476 (18)0.0145 (15)0.0134 (15)0.0047 (14)
C30.056 (2)0.0452 (18)0.0448 (18)0.0084 (15)0.0109 (15)0.0037 (13)
C40.069 (3)0.050 (2)0.052 (2)0.0161 (17)0.0058 (18)0.0008 (15)
C50.0546 (19)0.0457 (18)0.0469 (18)0.0120 (15)0.0039 (14)0.0064 (14)
C60.086 (3)0.0425 (18)0.0483 (19)0.0166 (17)0.0068 (18)0.0129 (14)
C70.075 (2)0.0394 (18)0.0488 (19)0.0030 (16)0.0113 (17)0.0109 (14)
C80.054 (2)0.062 (2)0.074 (2)0.0096 (17)0.0144 (18)0.0206 (19)
C90.052 (2)0.056 (2)0.064 (2)0.0173 (16)0.0065 (16)0.0242 (17)
C100.0511 (18)0.0340 (15)0.0363 (15)0.0081 (13)0.0005 (13)0.0036 (12)
C110.0485 (17)0.0352 (15)0.0388 (16)0.0074 (13)0.0004 (13)0.0027 (12)
C120.058 (2)0.0422 (18)0.075 (2)0.0093 (15)0.0158 (17)0.0178 (16)
C130.061 (2)0.048 (2)0.119 (4)0.0223 (18)0.023 (2)0.021 (2)
C140.059 (2)0.067 (3)0.128 (4)0.020 (2)0.042 (3)0.014 (3)
C150.063 (2)0.068 (3)0.092 (3)0.007 (2)0.036 (2)0.019 (2)
C160.0458 (18)0.0442 (18)0.060 (2)0.0015 (14)0.0130 (15)0.0110 (15)
C170.0369 (15)0.0309 (14)0.0500 (17)0.0014 (12)0.0059 (13)0.0030 (12)
C180.0565 (19)0.0324 (15)0.0491 (18)0.0057 (13)0.0039 (14)0.0028 (13)
C190.062 (2)0.0318 (16)0.070 (2)0.0099 (14)0.0058 (17)0.0056 (15)
C200.0493 (19)0.0436 (18)0.070 (2)0.0082 (15)0.0007 (16)0.0203 (16)
C210.0530 (19)0.059 (2)0.0478 (19)0.0066 (16)0.0035 (15)0.0129 (15)
C220.0494 (18)0.0381 (16)0.0468 (18)0.0054 (13)0.0006 (14)0.0023 (13)
C230.0358 (15)0.0320 (14)0.0412 (16)0.0007 (11)0.0057 (12)0.0075 (11)
C240.0501 (18)0.0340 (16)0.065 (2)0.0011 (14)0.0100 (15)0.0029 (14)
C250.060 (2)0.0307 (17)0.084 (3)0.0062 (15)0.0025 (19)0.0020 (16)
C260.056 (2)0.0448 (19)0.079 (3)0.0181 (16)0.0051 (18)0.0186 (17)
C270.0494 (19)0.063 (2)0.059 (2)0.0106 (16)0.0101 (16)0.0107 (17)
C280.0465 (17)0.0421 (17)0.0471 (18)0.0054 (14)0.0067 (14)0.0003 (13)
C290.0418 (16)0.0277 (14)0.0382 (15)0.0029 (11)0.0013 (12)0.0045 (11)
Geometric parameters (Å, º) top
Ni1—S2i2.1580 (10)C12—C131.374 (5)
Ni1—S22.1580 (10)C12—C171.391 (4)
Ni1—S12.1694 (10)C12—H120.9300
Ni1—S1i2.1694 (10)C13—C141.366 (6)
S1—C21.736 (4)C13—H130.9300
S2—C31.739 (3)C14—C151.372 (6)
N1—C11.140 (5)C14—H140.9300
N2—C41.139 (5)C15—C161.369 (5)
N3—O11.190 (5)C15—H150.9300
N3—O21.198 (6)C16—C171.383 (4)
N3—C71.477 (5)C16—H160.9300
O3—H3A0.8500C18—C191.385 (4)
O3—H3B0.8500C18—C231.386 (4)
P1—C171.786 (3)C18—H180.9300
P1—C231.795 (3)C19—C201.357 (5)
P1—C291.799 (3)C19—H190.9300
P1—C111.808 (3)C20—C211.378 (5)
C1—C21.433 (5)C20—H200.9300
C2—C31.350 (5)C21—C221.383 (4)
C3—C41.431 (5)C21—H210.9300
C5—C101.382 (4)C22—C231.381 (4)
C5—C61.389 (5)C22—H220.9300
C5—H50.9300C24—C291.381 (4)
C6—C71.365 (5)C24—C251.382 (5)
C6—H60.9300C24—H240.9300
C7—C81.363 (5)C25—C261.358 (5)
C8—C91.380 (5)C25—H250.9300
C8—H80.9300C26—C271.376 (5)
C9—C101.375 (5)C26—H260.9300
C9—H90.9300C27—C281.380 (5)
C10—C111.512 (4)C27—H270.9300
C11—H11A0.9700C28—C291.384 (4)
C11—H11B0.9700C28—H280.9300
S2i—Ni1—S2180.000 (1)C17—C12—H12120.2
S2i—Ni1—S188.13 (4)C14—C13—C12120.3 (4)
S2—Ni1—S191.87 (4)C14—C13—H13119.9
S2i—Ni1—S1i91.87 (4)C12—C13—H13119.9
S2—Ni1—S1i88.13 (4)C13—C14—C15120.3 (4)
S1—Ni1—S1i180.000 (1)C13—C14—H14119.9
C2—S1—Ni1103.51 (12)C15—C14—H14119.9
C3—S2—Ni1103.72 (11)C16—C15—C14120.4 (4)
O1—N3—O2123.8 (4)C16—C15—H15119.8
O1—N3—C7117.9 (4)C14—C15—H15119.8
O2—N3—C7118.3 (4)C15—C16—C17119.7 (3)
H3A—O3—H3B109.5C15—C16—H16120.1
C17—P1—C23111.45 (13)C17—C16—H16120.1
C17—P1—C29109.51 (13)C16—C17—C12119.6 (3)
C23—P1—C29108.34 (13)C16—C17—P1121.7 (2)
C17—P1—C11111.23 (14)C12—C17—P1118.7 (2)
C23—P1—C11107.19 (13)C19—C18—C23119.3 (3)
C29—P1—C11109.04 (14)C19—C18—H18120.4
N1—C1—C2178.1 (5)C23—C18—H18120.4
C3—C2—C1121.4 (3)C20—C19—C18120.9 (3)
C3—C2—S1120.4 (3)C20—C19—H19119.6
C1—C2—S1118.1 (3)C18—C19—H19119.6
C2—C3—C4123.2 (3)C19—C20—C21120.2 (3)
C2—C3—S2120.4 (3)C19—C20—H20119.9
C4—C3—S2116.3 (2)C21—C20—H20119.9
N2—C4—C3176.2 (4)C20—C21—C22119.7 (3)
C10—C5—C6119.8 (3)C20—C21—H21120.1
C10—C5—H5120.1C22—C21—H21120.1
C6—C5—H5120.1C23—C22—C21120.1 (3)
C7—C6—C5118.8 (3)C23—C22—H22119.9
C7—C6—H6120.6C21—C22—H22119.9
C5—C6—H6120.6C22—C23—C18119.7 (3)
C8—C7—C6122.5 (3)C22—C23—P1119.7 (2)
C8—C7—N3118.6 (4)C18—C23—P1120.6 (2)
C6—C7—N3118.9 (3)C29—C24—C25119.0 (3)
C7—C8—C9118.3 (3)C29—C24—H24120.5
C7—C8—H8120.9C25—C24—H24120.5
C9—C8—H8120.9C26—C25—C24121.2 (3)
C10—C9—C8121.0 (3)C26—C25—H25119.4
C10—C9—H9119.5C24—C25—H25119.4
C8—C9—H9119.5C25—C26—C27120.0 (3)
C9—C10—C5119.5 (3)C25—C26—H26120.0
C9—C10—C11119.0 (3)C27—C26—H26120.0
C5—C10—C11121.4 (3)C26—C27—C28119.9 (3)
C10—C11—P1116.2 (2)C26—C27—H27120.1
C10—C11—H11A108.2C28—C27—H27120.1
P1—C11—H11A108.2C27—C28—C29119.9 (3)
C10—C11—H11B108.2C27—C28—H28120.0
P1—C11—H11B108.2C29—C28—H28120.0
H11A—C11—H11B107.4C24—C29—C28120.0 (3)
C13—C12—C17119.7 (3)C24—C29—P1121.3 (2)
C13—C12—H12120.2C28—C29—P1118.6 (2)
Symmetry code: (i) x, y+1, z+2.
 

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