Literature DB >> 21583040

Bis[μ-2-(2-carboxyl-atophen-yl)acetato]-κO,O:O;κO:O,O-bis-[aqua-(1,10-phenanthroline-κN,N')nickel(II)].

Feng Li1, Huifang Zeng, Zhaowei Yan, Taohai Li.   

Abstract

The title compound, [Ni(2)(C(9)H(6)O(4))(2)(C(12)H(8)N(2))(2)(H(2)O)(2)], is isostructural with the Zn(II) analogue. Each Ni(II) atom is coordinated in a distorted octa-hedral geometry by three O atoms from two homophthalate anions, one aqua O atom and two 1,10-phenanthroline N atoms. The two Ni(II) atoms are linked by two bridging homophthalate dianions into a centrosymmetric dinuclear unit. The dinuclear units are linked into one-dimensional ladder-like chains along [100] by O-H⋯O hydrogen bonds between the coordinated water mol-ecules and one of the O atoms of the carboxyl-atomethyl group.

Entities:  

Year:  2009        PMID： 21583040      PMCID： PMC2969824          DOI： 10.1107/S1600536809018339

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


Related literature

For the ZnII analogue, see: He et al. (2006 ▶); Sun (2006 ▶).

Experimental

Crystal data

[Ni2(C9H6O4)2(C12H8N2)2(H2O)2] M = 870.14 Monoclinic, a = 8.819 (3) Å b = 19.432 (6) Å c = 12.898 (3) Å β = 122.900 (17)° V = 1855.8 (10) Å3 Z = 2 Mo Kα radiation μ = 1.08 mm−1 T = 173 K 0.45 × 0.40 × 0.20 mm

Data collection

Rigaku Mercury70 CCD diffractometer Absorption correction: multi-scan (CrystalClear; Molecular Structure Corporation & Rigaku, 2001 ▶) T min = 0.618, T max = 0.806 14201 measured reflections 4232 independent reflections 3900 reflections with I > 2σ(I) R int = 0.021

Refinement

R[F 2 > 2σ(F 2)] = 0.032 wR(F 2) = 0.083 S = 1.05 4232 reflections 262 parameters H-atom parameters constrained Δρmax = 0.43 e Å−3 Δρmin = −0.35 e Å−3 Data collection: CrystalClear (Molecular Structure Corporation & Rigaku, 2001 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; 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: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809018339/bi2368sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809018339/bi2368Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ni2(C9H6O4)2(C12H8N2)2(H2O)2]F(000) = 896
Mr = 870.14Dx = 1.557 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5071 reflections
a = 8.819 (3) Åθ = 3.1–27.5°
b = 19.432 (6) ŵ = 1.08 mm−1
c = 12.898 (3) ÅT = 173 K
β = 122.900 (17)°Prism, green
V = 1855.8 (10) Å30.45 × 0.40 × 0.20 mm
Z = 2
Rigaku Mercury70 CCD diffractometer4232 independent reflections
Radiation source: fine-focus sealed tube3900 reflections with I > 2σ(I)
graphiteRint = 0.021
φ scansθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan (CrystalClear; Molecular Structure Corporation & Rigaku, 2001)h = −11→10
Tmin = 0.618, Tmax = 0.806k = −25→25
14201 measured reflectionsl = −8→16
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.083H-atom parameters constrained
S = 1.05w = 1/[σ2(Fo2) + (0.0409P)2 + 0.7079P] where P = (Fo2 + 2Fc2)/3
4232 reflections(Δ/σ)max = 0.001
262 parametersΔρmax = 0.43 e Å−3
0 restraintsΔρmin = −0.35 e Å−3
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*/Ueq
Ni10.44081 (3)−0.039291 (11)0.673702 (19)0.03024 (8)
O1−0.33605 (19)0.17448 (7)0.51356 (14)0.0502 (4)
N10.6408 (2)0.03318 (7)0.77780 (14)0.0345 (3)
C1−0.2231 (2)0.15639 (8)0.48860 (15)0.0314 (3)
O2−0.25662 (17)0.11526 (7)0.40350 (12)0.0435 (3)
N20.52689 (19)−0.07298 (7)0.84877 (13)0.0340 (3)
C2−0.0352 (2)0.18683 (8)0.56453 (15)0.0304 (3)
O30.23654 (17)0.03212 (6)0.64245 (12)0.0364 (3)
C3−0.0064 (3)0.23714 (9)0.65075 (17)0.0400 (4)
H3−0.10370.25020.65840.048*
O40.31651 (16)0.02133 (6)0.50972 (11)0.0348 (3)
C40.1591 (3)0.26839 (10)0.72498 (19)0.0497 (5)
H40.17610.30150.78470.060*
C50.2996 (3)0.25140 (11)0.7122 (2)0.0534 (5)
H50.41330.27360.76130.064*
C60.2739 (3)0.20201 (11)0.6275 (2)0.0485 (5)
H60.37150.19080.61900.058*
C70.1087 (2)0.16760 (9)0.55342 (16)0.0340 (4)
C80.1050 (2)0.11111 (10)0.47180 (16)0.0389 (4)
H8A−0.02040.09440.41690.047*
H8B0.14510.12990.41920.047*
C90.2252 (2)0.05161 (9)0.54613 (16)0.0306 (3)
C100.6981 (3)0.08452 (10)0.74036 (19)0.0448 (4)
H100.64410.09100.65420.054*
C110.8343 (3)0.12948 (11)0.8218 (2)0.0521 (5)
H110.87140.16590.79130.062*
C120.9141 (3)0.12072 (11)0.9459 (2)0.0483 (5)
H121.00710.15111.00240.058*
C130.8583 (2)0.06661 (10)0.99009 (17)0.0390 (4)
C140.9333 (3)0.05242 (11)1.11804 (19)0.0475 (5)
H141.02840.08061.17880.057*
C150.8722 (3)0.00016 (11)1.15414 (17)0.0472 (5)
H150.9228−0.00731.23970.057*
C160.7318 (3)−0.04433 (9)1.06539 (17)0.0386 (4)
C170.6650 (3)−0.10109 (11)1.09668 (18)0.0473 (5)
H170.7111−0.11121.18080.057*
C180.5337 (3)−0.14141 (11)1.00544 (19)0.0496 (5)
H180.4877−0.17981.02560.060*
C190.4669 (3)−0.12587 (10)0.88166 (18)0.0428 (4)
H190.3752−0.15430.81900.051*
C200.7199 (2)0.02413 (9)0.90086 (16)0.0323 (3)
C210.6584 (2)−0.03289 (8)0.94044 (16)0.0320 (3)
O1W0.60875 (16)−0.09246 (6)0.63816 (12)0.0362 (3)
H1WA0.5459−0.12310.58680.060*
H1WB0.6287−0.06860.59350.038*
U11U22U33U12U13U23
Ni10.02846 (13)0.03614 (13)0.02636 (13)−0.00226 (8)0.01504 (10)−0.00119 (8)
O10.0441 (8)0.0540 (8)0.0621 (9)−0.0049 (6)0.0350 (7)−0.0166 (7)
N10.0306 (7)0.0422 (8)0.0293 (7)−0.0014 (6)0.0153 (6)0.0026 (6)
C10.0342 (8)0.0300 (7)0.0306 (8)−0.0002 (6)0.0181 (7)0.0024 (6)
O20.0400 (7)0.0534 (8)0.0438 (8)−0.0164 (6)0.0272 (6)−0.0193 (6)
N20.0342 (7)0.0387 (7)0.0302 (7)−0.0011 (6)0.0181 (6)0.0004 (6)
C20.0357 (8)0.0257 (7)0.0281 (8)−0.0009 (6)0.0162 (7)0.0020 (6)
O30.0403 (7)0.0432 (6)0.0314 (6)0.0010 (5)0.0231 (6)−0.0005 (5)
C30.0523 (11)0.0305 (8)0.0396 (10)−0.0026 (7)0.0265 (9)−0.0046 (7)
O40.0327 (6)0.0443 (6)0.0325 (6)0.0047 (5)0.0211 (5)0.0013 (5)
C40.0623 (13)0.0335 (9)0.0437 (11)−0.0103 (9)0.0226 (10)−0.0102 (8)
C50.0465 (11)0.0453 (10)0.0509 (12)−0.0151 (9)0.0151 (10)−0.0049 (9)
C60.0356 (10)0.0530 (11)0.0516 (12)−0.0046 (8)0.0203 (9)−0.0003 (10)
C70.0339 (8)0.0347 (8)0.0304 (8)0.0009 (6)0.0154 (7)0.0032 (7)
C80.0343 (9)0.0526 (10)0.0292 (9)0.0098 (8)0.0169 (8)0.0005 (8)
C90.0259 (8)0.0381 (8)0.0276 (8)−0.0046 (6)0.0145 (7)−0.0063 (7)
C100.0437 (10)0.0504 (10)0.0389 (10)−0.0055 (8)0.0214 (9)0.0057 (8)
C110.0544 (12)0.0495 (11)0.0546 (13)−0.0147 (9)0.0311 (11)−0.0018 (10)
C120.0457 (11)0.0481 (11)0.0502 (12)−0.0130 (9)0.0254 (10)−0.0132 (9)
C130.0345 (9)0.0448 (9)0.0363 (10)−0.0027 (7)0.0184 (8)−0.0095 (8)
C140.0440 (11)0.0577 (12)0.0330 (10)−0.0044 (9)0.0158 (9)−0.0140 (9)
C150.0497 (11)0.0617 (12)0.0252 (9)0.0009 (9)0.0170 (8)−0.0058 (8)
C160.0401 (10)0.0478 (10)0.0302 (9)0.0060 (8)0.0206 (8)0.0002 (7)
C170.0564 (12)0.0577 (12)0.0330 (10)0.0054 (10)0.0276 (10)0.0077 (9)
C180.0598 (13)0.0514 (11)0.0442 (11)−0.0019 (9)0.0325 (10)0.0096 (9)
C190.0454 (10)0.0456 (10)0.0392 (10)−0.0060 (8)0.0242 (9)0.0023 (8)
C200.0274 (8)0.0397 (8)0.0289 (8)0.0011 (6)0.0148 (7)−0.0018 (7)
C210.0284 (8)0.0374 (8)0.0308 (9)0.0036 (6)0.0165 (7)−0.0021 (7)
O1W0.0328 (6)0.0400 (6)0.0381 (7)0.0055 (5)0.0207 (6)0.0077 (5)
Ni1—O2i2.0130 (13)C7—C81.509 (2)
Ni1—O1W2.0515 (13)C8—C91.508 (2)
Ni1—N22.0595 (15)C8—H8A0.990
Ni1—N12.0794 (16)C8—H8B0.990
Ni1—O42.1316 (13)C10—C111.393 (3)
Ni1—O32.1319 (14)C10—H100.950
O1—C11.252 (2)C11—C121.365 (3)
N1—C101.323 (2)C11—H110.950
N1—C201.354 (2)C12—C131.406 (3)
C1—O21.256 (2)C12—H120.950
C1—C21.514 (2)C13—C201.403 (2)
O2—Ni1i2.0130 (13)C13—C141.432 (3)
N2—C191.327 (2)C14—C151.346 (3)
N2—C211.364 (2)C14—H140.950
C2—C31.397 (2)C15—C161.432 (3)
C2—C71.403 (2)C15—H150.950
O3—C91.250 (2)C16—C211.390 (3)
C3—C41.377 (3)C16—C171.409 (3)
C3—H30.950C17—C181.363 (3)
O4—C91.275 (2)C17—H170.950
C4—C51.376 (3)C18—C191.402 (3)
C4—H40.950C18—H180.950
C5—C61.377 (3)C19—H190.950
C5—H50.950C20—C211.443 (2)
C6—C71.404 (3)O1W—H1WA0.837
C6—H60.950O1W—H1WB0.828
O2i—Ni1—O1W90.38 (6)C7—C8—H8A109.2
O2i—Ni1—N291.55 (6)C9—C8—H8B109.2
O1W—Ni1—N2101.77 (6)C7—C8—H8B109.2
O2i—Ni1—N1171.71 (6)H8A—C8—H8B107.9
O1W—Ni1—N191.33 (6)O3—C9—O4120.04 (16)
N2—Ni1—N180.16 (6)O3—C9—C8120.90 (15)
O2i—Ni1—O494.16 (6)O4—C9—C8119.06 (15)
O1W—Ni1—O495.81 (5)N1—C10—C11122.82 (19)
N2—Ni1—O4161.47 (5)N1—C10—H10118.6
N1—Ni1—O493.73 (6)C11—C10—H10118.6
O2i—Ni1—O390.68 (6)C12—C11—C10119.36 (19)
O1W—Ni1—O3157.53 (5)C12—C11—H11120.3
N2—Ni1—O3100.64 (5)C10—C11—H11120.3
N1—Ni1—O390.83 (6)C11—C12—C13119.84 (18)
O4—Ni1—O361.73 (5)C11—C12—H12120.1
C10—N1—C20118.06 (16)C13—C12—H12120.1
C10—N1—Ni1129.31 (13)C20—C13—C12116.59 (17)
C20—N1—Ni1112.64 (11)C20—C13—C14118.91 (18)
O1—C1—O2124.09 (16)C12—C13—C14124.50 (18)
O1—C1—C2117.91 (15)C15—C14—C13121.51 (18)
O2—C1—C2118.00 (15)C15—C14—H14119.2
C1—O2—Ni1i129.98 (11)C13—C14—H14119.2
C19—N2—C21117.66 (16)C14—C15—C16120.91 (18)
C19—N2—Ni1128.56 (13)C14—C15—H15119.5
C21—N2—Ni1113.73 (11)C16—C15—H15119.5
C3—C2—C7118.98 (16)C21—C16—C17116.94 (18)
C3—C2—C1116.77 (15)C21—C16—C15119.12 (17)
C7—C2—C1124.25 (15)C17—C16—C15123.92 (18)
C9—O3—Ni189.34 (10)C18—C17—C16119.59 (18)
C4—C3—C2121.85 (18)C18—C17—H17120.2
C4—C3—H3119.1C16—C17—H17120.2
C2—C3—H3119.1C17—C18—C19119.58 (19)
C9—O4—Ni188.68 (10)C17—C18—H18120.2
C5—C4—C3119.61 (19)C19—C18—H18120.2
C5—C4—H4120.2N2—C19—C18122.49 (18)
C3—C4—H4120.2N2—C19—H19118.8
C4—C5—C6119.43 (19)C18—C19—H19118.8
C4—C5—H5120.3N1—C20—C13123.33 (16)
C6—C5—H5120.3N1—C20—C21117.46 (15)
C5—C6—C7122.33 (19)C13—C20—C21119.21 (16)
C5—C6—H6118.8N2—C21—C16123.73 (16)
C7—C6—H6118.8N2—C21—C20115.96 (15)
C2—C7—C6117.74 (17)C16—C21—C20120.31 (16)
C2—C7—C8125.94 (16)Ni1—O1W—H1WA106.6
C6—C7—C8116.28 (16)Ni1—O1W—H1WB109.0
C9—C8—C7111.88 (14)H1WA—O1W—H1WB98.5
C9—C8—H8A109.2
O1W—Ni1—N1—C1076.39 (17)C2—C7—C8—C9−112.08 (19)
N2—Ni1—N1—C10178.11 (18)C6—C7—C8—C965.6 (2)
O4—Ni1—N1—C10−19.52 (17)Ni1—O3—C9—O44.62 (16)
O3—Ni1—N1—C10−81.24 (17)Ni1—O3—C9—C8−175.03 (14)
O1W—Ni1—N1—C20−103.35 (12)Ni1—O4—C9—O3−4.62 (16)
N2—Ni1—N1—C20−1.63 (12)Ni1—O4—C9—C8175.04 (14)
O4—Ni1—N1—C20160.74 (12)C7—C8—C9—O338.4 (2)
O3—Ni1—N1—C2099.02 (12)C7—C8—C9—O4−141.28 (16)
O1—C1—O2—Ni1i−26.5 (3)C20—N1—C10—C11−0.5 (3)
C2—C1—O2—Ni1i154.47 (12)Ni1—N1—C10—C11179.76 (15)
O2i—Ni1—N2—C19−0.48 (16)N1—C10—C11—C120.3 (3)
O1W—Ni1—N2—C19−91.19 (16)C10—C11—C12—C130.0 (3)
N1—Ni1—N2—C19179.50 (17)C11—C12—C13—C20−0.2 (3)
O4—Ni1—N2—C19107.5 (2)C11—C12—C13—C14179.5 (2)
O3—Ni1—N2—C1990.51 (16)C20—C13—C14—C15−1.0 (3)
O2i—Ni1—N2—C21−177.86 (12)C12—C13—C14—C15179.2 (2)
O1W—Ni1—N2—C2191.43 (12)C13—C14—C15—C161.4 (3)
N1—Ni1—N2—C212.12 (11)C14—C15—C16—C21−0.1 (3)
O4—Ni1—N2—C21−69.8 (2)C14—C15—C16—C17178.2 (2)
O3—Ni1—N2—C21−86.87 (12)C21—C16—C17—C18−0.2 (3)
O1—C1—C2—C3−4.9 (2)C15—C16—C17—C18−178.54 (19)
O2—C1—C2—C3174.24 (16)C16—C17—C18—C190.0 (3)
O1—C1—C2—C7175.03 (16)C21—N2—C19—C18−0.1 (3)
O2—C1—C2—C7−5.9 (2)Ni1—N2—C19—C18−177.39 (15)
O2i—Ni1—O3—C9−97.07 (10)C17—C18—C19—N20.2 (3)
O1W—Ni1—O3—C9−4.43 (19)C10—N1—C20—C130.4 (3)
N2—Ni1—O3—C9171.22 (10)Ni1—N1—C20—C13−179.87 (13)
N1—Ni1—O3—C991.08 (11)C10—N1—C20—C21−178.83 (16)
O4—Ni1—O3—C9−2.71 (9)Ni1—N1—C20—C210.94 (19)
C7—C2—C3—C40.0 (3)C12—C13—C20—N10.0 (3)
C1—C2—C3—C4179.96 (16)C14—C13—C20—N1−179.76 (17)
O2i—Ni1—O4—C991.19 (10)C12—C13—C20—C21179.15 (16)
O1W—Ni1—O4—C9−178.00 (10)C14—C13—C20—C21−0.6 (3)
N2—Ni1—O4—C9−16.4 (2)C19—N2—C21—C16−0.2 (3)
N1—Ni1—O4—C9−86.27 (10)Ni1—N2—C21—C16177.54 (13)
O3—Ni1—O4—C92.66 (9)C19—N2—C21—C20−179.95 (15)
C2—C3—C4—C51.9 (3)Ni1—N2—C21—C20−2.26 (18)
C3—C4—C5—C6−1.7 (3)C17—C16—C21—N20.3 (3)
C4—C5—C6—C7−0.4 (3)C15—C16—C21—N2178.70 (17)
C3—C2—C7—C6−2.1 (2)C17—C16—C21—C20−179.90 (16)
C1—C2—C7—C6178.01 (16)C15—C16—C21—C20−1.5 (3)
C3—C2—C7—C8175.58 (16)N1—C20—C21—N20.9 (2)
C1—C2—C7—C8−4.3 (3)C13—C20—C21—N2−178.35 (15)
C5—C6—C7—C22.3 (3)N1—C20—C21—C16−178.93 (16)
C5—C6—C7—C8−175.61 (19)C13—C20—C21—C161.8 (2)
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O1i0.841.872.653 (2)155
O1W—H1WB···O4ii0.831.882.7108 (17)175
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1W—H1WA⋯O1i0.841.872.653 (2)155
O1W—H1WB⋯O4ii0.831.882.7108 (17)175

Symmetry codes: (i) ; (ii) .

  1 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290
  1 in total
  1 in total

1.  Bis(μ-biphenyl-2,2'-dicarboxyl-ato)bis-[aqua-(4,4'-dimethyl-2,2'-bipyridine-κN,N')copper(II)].

Authors:  Xi-Yan Dong; Xiao-Jie Xu; Lei Yang
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-10-17
  1 in total

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