Literature DB >> 21580849

Tetra-kis[tris-(2,2'-bi-1H-benzimidazole)nickel(II)] bis-(phosphate) sulfate.

Chun-Sheng Ling1, Lin Yan.   

Abstract

The title compound, [Ni(C(14)H(10)N(4))(3)](4)(PO(4))(2)(SO(4)), consists of [Ni(C(14)H(10)N(4))(3)](2+) complex cations (.3. symmetry) and disordered anions ( symmetry) with occupancy factors of two-thirds for PO(4) (3-) and one-third for SO(4) (2-). The Ni(2+) centre is chelated by three bidentate 2,2'-bi-1H-benzimidazole mol-ecules in a distorted octa-hedral coordination. N-H⋯O hydrogen bonds consolidate the building units into a framework structure.

Entities:  

Year:  2008        PMID： 21580849      PMCID： PMC2959627          DOI： 10.1107/S1600536808032571

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For the potential applications of metal–organic coordination compounds in gas absorption and separation, catalysis, non-linear optics, luminescence and magnetism, see: Kitagawa & Matsuda (2007 ▶); Maspoch et al. (2007 ▶).

Experimental

Crystal data

[Ni(C14H10N4)3]4(PO4)2(SO4) M = 3331.96 Cubic, a = 24.964 (7) Å V = 15558 (8) Å3 Z = 4 Mo Kα radiation μ = 0.59 mm−1 T = 296 (2) K 0.32 × 0.27 × 0.23 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2001 ▶) T min = 0.834, T max = 0.876 20222 measured reflections 2551 independent reflections 1782 reflections with I > 2σ(I) R int = 0.066

Refinement

R[F 2 > 2σ(F 2)] = 0.038 wR(F 2) = 0.098 S = 1.01 2551 reflections 177 parameters H-atom parameters constrained Δρmax = 0.61 e Å−3 Δρmin = −0.20 e Å−3 Absolute structure: Flack (1983 ▶), 1182 Friedel pairs Flack parameter: −0.02 (2) Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808032571/at2642sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808032571/at2642Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ni(C14H10N4)3]4(PO4)2(SO4)Dx = 1.423 Mg m−3
Mr = 3331.96Mo Kα radiation, λ = 0.71073 Å
Cubic, I43dCell parameters from 3375 reflections
Hall symbol: I -4bd 2c 3θ = 2.3–19.2°
a = 24.964 (7) ŵ = 0.59 mm−1
V = 15558 (8) Å3T = 296 K
Z = 4Block, green
F(000) = 68720.32 × 0.27 × 0.23 mm
Bruker SMART CCD area-detector diffractometer2551 independent reflections
Radiation source: fine-focus sealed tube1782 reflections with I > 2σ(I)
graphiteRint = 0.066
φ and ω scansθmax = 26.0°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 2001)h = −30→11
Tmin = 0.834, Tmax = 0.876k = −30→29
20222 measured reflectionsl = −21→20
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.038H-atom parameters constrained
wR(F2) = 0.098w = 1/[σ2(Fo2) + (0.0528P)2] where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.001
2551 reflectionsΔρmax = 0.61 e Å−3
177 parametersΔρmin = −0.20 e Å−3
0 restraintsAbsolute structure: Flack (1983), 1182 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: −0.02 (2)
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.
xyzUiso*/UeqOcc. (<1)
Ni10.564621 (16)0.435379 (16)−0.064621 (16)0.0428 (2)
P10.75000.62501.00000.0427 (4)0.67
S10.75000.62501.00000.0427 (4)0.33
N10.64773 (10)0.44469 (11)−0.06574 (11)0.0443 (6)
N20.71668 (10)0.50117 (12)−0.06248 (11)0.0498 (7)
H2B0.73400.5309−0.06040.060*
N30.56297 (10)0.42828 (11)0.02009 (10)0.0444 (6)
N40.55652 (11)0.37290 (12)0.08942 (11)0.0502 (7)
H4B0.55380.34350.10720.060*
C10.69498 (13)0.41559 (13)−0.06917 (13)0.0462 (8)
C20.70405 (15)0.36114 (16)−0.07434 (15)0.0594 (9)
H20.67580.3370−0.07630.071*
C30.75637 (17)0.34409 (18)−0.07642 (16)0.0744 (13)
H30.76380.3077−0.07970.089*
C40.79858 (16)0.3808 (2)−0.07359 (16)0.0707 (12)
H40.83350.3679−0.07500.085*
C50.79104 (13)0.43383 (18)−0.06895 (15)0.0627 (10)
H50.81970.4576−0.06700.075*
C60.73810 (12)0.45147 (14)−0.06724 (14)0.0473 (8)
C70.66286 (13)0.49523 (14)−0.06164 (13)0.0443 (8)
C80.56226 (15)0.45873 (13)0.06673 (14)0.0487 (9)
C90.56566 (17)0.51278 (15)0.07424 (15)0.0645 (11)
H90.56810.53630.04550.077*
C100.5653 (2)0.53090 (18)0.12671 (19)0.0848 (13)
H100.56720.56750.13330.102*
C110.5623 (2)0.49628 (19)0.16920 (17)0.0863 (14)
H110.56270.51020.20370.104*
C120.55859 (18)0.44183 (18)0.16272 (14)0.0698 (11)
H120.55620.41860.19170.084*
C130.55865 (13)0.42369 (14)0.11042 (13)0.0489 (8)
C140.55946 (13)0.37792 (14)0.03571 (13)0.0443 (8)
O10.77314 (11)0.59036 (9)0.95604 (10)0.0629 (7)
U11U22U33U12U13U23
Ni10.0428 (2)0.0428 (2)0.0428 (2)−0.00140 (19)−0.00140 (19)0.00140 (19)
P10.0469 (6)0.0341 (9)0.0469 (6)0.0000.0000.000
S10.0469 (6)0.0341 (9)0.0469 (6)0.0000.0000.000
N10.0386 (14)0.0485 (17)0.0458 (16)0.0000 (13)−0.0006 (13)0.0019 (15)
N20.0447 (17)0.0543 (18)0.0503 (17)−0.0083 (14)−0.0009 (14)−0.0019 (15)
N30.0432 (16)0.0445 (16)0.0456 (15)0.0006 (15)−0.0046 (13)−0.0007 (13)
N40.0552 (19)0.0518 (18)0.0436 (17)−0.0046 (14)−0.0034 (14)0.0093 (14)
C10.049 (2)0.0486 (19)0.0411 (18)0.0030 (16)−0.0031 (17)−0.0036 (15)
C20.054 (2)0.060 (2)0.065 (2)0.0073 (18)−0.0023 (19)−0.0042 (19)
C30.064 (3)0.076 (3)0.084 (3)0.024 (2)−0.003 (2)−0.009 (2)
C40.045 (2)0.097 (4)0.070 (3)0.021 (2)−0.002 (2)−0.014 (2)
C50.0439 (19)0.083 (3)0.061 (3)0.000 (2)−0.0050 (18)−0.016 (3)
C60.0417 (19)0.064 (2)0.0366 (18)0.0018 (16)−0.0048 (16)−0.0077 (17)
C70.044 (2)0.048 (2)0.0410 (19)−0.0065 (15)−0.0027 (15)−0.0012 (16)
C80.049 (2)0.052 (2)0.0449 (19)0.0051 (16)−0.0042 (18)−0.0057 (16)
C90.092 (3)0.050 (2)0.051 (2)−0.002 (2)−0.009 (2)−0.0036 (17)
C100.124 (4)0.065 (3)0.066 (3)0.006 (3)−0.010 (3)−0.013 (2)
C110.133 (4)0.077 (3)0.049 (3)0.001 (3)−0.013 (3)−0.017 (2)
C120.093 (3)0.074 (3)0.042 (2)−0.006 (3)−0.005 (2)0.001 (2)
C130.050 (2)0.055 (2)0.0423 (19)−0.0009 (18)−0.0050 (16)−0.0006 (16)
C140.0315 (18)0.053 (2)0.049 (2)−0.0032 (16)−0.0021 (15)0.0045 (17)
O10.0818 (18)0.0455 (15)0.0616 (17)−0.0077 (13)0.0150 (14)−0.0033 (12)
Ni1—N12.088 (3)C1—C61.401 (5)
Ni1—N1i2.088 (3)C2—C31.375 (5)
Ni1—N1ii2.088 (3)C2—H20.9300
Ni1—N3ii2.122 (3)C3—C41.398 (6)
Ni1—N32.122 (3)C3—H30.9300
Ni1—N3i2.122 (3)C4—C51.342 (6)
P1—O1iii1.512 (3)C4—H40.9300
P1—O1iv1.512 (3)C5—C61.394 (4)
P1—O11.512 (3)C5—H50.9300
P1—O1v1.512 (3)C7—C14ii1.435 (5)
N1—C71.321 (4)C8—C91.365 (5)
N1—C11.388 (4)C8—C131.401 (5)
N2—C71.352 (4)C9—C101.386 (6)
N2—C61.356 (4)C9—H90.9300
N2—H2B0.8600C10—C111.370 (6)
N3—C141.319 (4)C10—H100.9300
N3—C81.391 (4)C11—C121.372 (6)
N4—C141.349 (4)C11—H110.9300
N4—C131.373 (4)C12—C131.382 (5)
N4—H4B0.8600C12—H120.9300
C1—C21.384 (5)C14—C7i1.435 (5)
N1—Ni1—N1i95.67 (10)C1—C2—H2121.2
N1—Ni1—N1ii95.67 (10)C2—C3—C4120.7 (4)
N1i—Ni1—N1ii95.67 (10)C2—C3—H3119.6
N1—Ni1—N3ii78.84 (10)C4—C3—H3119.6
N1i—Ni1—N3ii170.67 (9)C5—C4—C3123.0 (4)
N1ii—Ni1—N3ii92.40 (9)C5—C4—H4118.5
N1—Ni1—N392.40 (9)C3—C4—H4118.5
N1i—Ni1—N378.84 (10)C4—C5—C6116.6 (4)
N1ii—Ni1—N3170.67 (9)C4—C5—H5121.7
N3ii—Ni1—N393.75 (9)C6—C5—H5121.7
N1—Ni1—N3i170.67 (9)N2—C6—C5131.7 (3)
N1i—Ni1—N3i92.40 (9)N2—C6—C1106.6 (3)
N1ii—Ni1—N3i78.84 (10)C5—C6—C1121.7 (3)
N3ii—Ni1—N3i93.75 (9)N1—C7—N2112.8 (3)
N3—Ni1—N3i93.75 (9)N1—C7—C14ii118.2 (3)
O1iii—P1—O1iv110.22 (17)N2—C7—C14ii128.9 (3)
O1iii—P1—O1109.10 (9)C9—C8—N3130.9 (3)
O1iv—P1—O1109.10 (9)C9—C8—C13121.0 (3)
O1iii—P1—O1v109.10 (9)N3—C8—C13108.1 (3)
O1iv—P1—O1v109.10 (9)C8—C9—C10116.9 (4)
O1—P1—O1v110.22 (17)C8—C9—H9121.6
C7—N1—C1105.2 (3)C10—C9—H9121.6
C7—N1—Ni1112.9 (2)C11—C10—C9121.7 (4)
C1—N1—Ni1141.9 (2)C11—C10—H10119.1
C7—N2—C6107.0 (3)C9—C10—H10119.1
C7—N2—H2B126.5C10—C11—C12122.5 (4)
C6—N2—H2B126.5C10—C11—H11118.7
C14—N3—C8105.8 (3)C12—C11—H11118.7
C14—N3—Ni1112.0 (2)C11—C12—C13115.8 (4)
C8—N3—Ni1142.1 (2)C11—C12—H12122.1
C14—N4—C13107.0 (3)C13—C12—H12122.1
C14—N4—H4B126.5N4—C13—C12131.5 (3)
C13—N4—H4B126.5N4—C13—C8106.4 (3)
C2—C1—N1131.2 (3)C12—C13—C8122.1 (3)
C2—C1—C6120.4 (3)N3—C14—N4112.7 (3)
N1—C1—C6108.4 (3)N3—C14—C7i117.7 (3)
C3—C2—C1117.6 (4)N4—C14—C7i129.5 (3)
C3—C2—H2121.2
N1i—Ni1—N1—C7−168.5 (2)C2—C1—C6—N2179.6 (3)
N1ii—Ni1—N1—C795.2 (3)N1—C1—C6—N20.3 (4)
N3ii—Ni1—N1—C73.9 (2)C2—C1—C6—C5−1.8 (5)
N3—Ni1—N1—C7−89.5 (3)N1—C1—C6—C5178.9 (3)
N3i—Ni1—N1—C741.7 (7)C1—N1—C7—N20.4 (4)
N1i—Ni1—N1—C111.1 (4)Ni1—N1—C7—N2−179.9 (2)
N1ii—Ni1—N1—C1−85.2 (3)C1—N1—C7—C14ii177.6 (3)
N3ii—Ni1—N1—C1−176.5 (4)Ni1—N1—C7—C14ii−2.6 (4)
N3—Ni1—N1—C190.1 (4)C6—N2—C7—N1−0.2 (4)
N3i—Ni1—N1—C1−138.6 (6)C6—N2—C7—C14ii−177.1 (3)
N1—Ni1—N3—C14−100.0 (2)C14—N3—C8—C9178.8 (4)
N1i—Ni1—N3—C14−4.7 (2)Ni1—N3—C8—C9−4.5 (7)
N1ii—Ni1—N3—C1449.9 (7)C14—N3—C8—C130.5 (4)
N3ii—Ni1—N3—C14−178.9 (2)Ni1—N3—C8—C13177.2 (3)
N3i—Ni1—N3—C1487.1 (3)N3—C8—C9—C10−178.2 (4)
N1—Ni1—N3—C883.5 (4)C13—C8—C9—C100.0 (6)
N1i—Ni1—N3—C8178.8 (4)C8—C9—C10—C110.7 (7)
N1ii—Ni1—N3—C8−126.7 (6)C9—C10—C11—C12−1.0 (8)
N3ii—Ni1—N3—C84.5 (4)C10—C11—C12—C130.6 (8)
N3i—Ni1—N3—C8−89.5 (3)C14—N4—C13—C12−178.1 (4)
C7—N1—C1—C2−179.6 (4)C14—N4—C13—C80.8 (4)
Ni1—N1—C1—C20.7 (7)C11—C12—C13—N4178.7 (4)
C7—N1—C1—C6−0.4 (4)C11—C12—C13—C80.0 (6)
Ni1—N1—C1—C6180.0 (3)C9—C8—C13—N4−179.3 (3)
N1—C1—C2—C3−179.6 (3)N3—C8—C13—N4−0.8 (4)
C6—C1—C2—C31.2 (5)C9—C8—C13—C12−0.3 (6)
C1—C2—C3—C4−0.3 (6)N3—C8—C13—C12178.2 (4)
C2—C3—C4—C5−0.2 (6)C8—N3—C14—N40.0 (4)
C3—C4—C5—C6−0.3 (6)Ni1—N3—C14—N4−177.9 (2)
C7—N2—C6—C5−178.5 (4)C8—N3—C14—C7i−177.4 (3)
C7—N2—C6—C10.0 (4)Ni1—N3—C14—C7i4.8 (3)
C4—C5—C6—N2179.5 (4)C13—N4—C14—N3−0.5 (4)
C4—C5—C6—C11.3 (6)C13—N4—C14—C7i176.5 (3)
D—H···AD—HH···AD···AD—H···A
N4—H4B···O1vi0.861.962.766 (4)156
N2—H2B···O1vii0.861.822.675 (4)170
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
N4—H4B⋯O1i0.861.962.766 (4)156
N2—H2B⋯O1ii0.861.822.675 (4)170

Symmetry codes: (i) ; (ii) .

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