Literature DB >> 21522299

Bis(N-nitroso-N-phenyl-hydroxy-laminato-κO,O')(1,10-phenanthroline-κN,N')lead(II).

Ezzatollah Najafi, Mostafa M Amini, Seik Weng Ng.   

Abstract

The two cupferronate ions and the N-heterocycle in the mononuclear title compound, [Pb(C(6)H(5)N(2)O(2))(2)(C(12)H(8)N(2))], O,O'- and N,N'-chelate to the Pb(II) atom, the geometry of which is a distorted Ψ-penta-gonal bipyramid.

Entities:  

Year:  2011        PMID: 21522299      PMCID: PMC3052161          DOI: 10.1107/S1600536811006787

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


Related literature

For the structure of dinuclear [Pb(C6H5N2O2)2]2, see: Najafi et al. (2011 ▶).

Experimental

Crystal data

[Pb(C6H5N2O2)2(C12H8N2)] M = 661.63 Monoclinic, a = 7.7033 (4) Å b = 15.9948 (8) Å c = 18.8929 (10) Å β = 100.919 (1)° V = 2285.7 (2) Å3 Z = 4 Mo Kα radiation μ = 7.43 mm−1 T = 100 K 0.20 × 0.10 × 0.10 mm

Data collection

Bruker SMART APEX diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.318, T max = 0.524 21418 measured reflections 5233 independent reflections 4676 reflections with I > 2σ(I) R int = 0.028

Refinement

R[F 2 > 2σ(F 2)] = 0.018 wR(F 2) = 0.047 S = 0.91 5233 reflections 316 parameters H-atom parameters constrained Δρmax = 0.74 e Å−3 Δρmin = −0.53 e Å−3 Data collection: APEX2 (Bruker, 2009 ▶); cell refinement: SAINT (Bruker, 2009 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811006787/bt5481sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536811006787/bt5481Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Pb(C6H5N2O2)2(C12H8N2)]F(000) = 1272
Mr = 661.63Dx = 1.923 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9896 reflections
a = 7.7033 (4) Åθ = 2.2–28.3°
b = 15.9948 (8) ŵ = 7.43 mm1
c = 18.8929 (10) ÅT = 100 K
β = 100.919 (1)°Prism, brown
V = 2285.7 (2) Å30.20 × 0.10 × 0.10 mm
Z = 4
Bruker SMART APEX diffractometer5233 independent reflections
Radiation source: fine-focus sealed tube4676 reflections with I > 2σ(I)
graphiteRint = 0.028
ω scansθmax = 27.5°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −9→10
Tmin = 0.318, Tmax = 0.524k = −20→18
21418 measured reflectionsl = −24→24
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.018Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.047H-atom parameters constrained
S = 0.91w = 1/[σ2(Fo2) + (0.0315P)2 + 1.0382P] where P = (Fo2 + 2Fc2)/3
5233 reflections(Δ/σ)max = 0.001
316 parametersΔρmax = 0.74 e Å3
0 restraintsΔρmin = −0.53 e Å3
xyzUiso*/Ueq
Pb10.545412 (12)0.564925 (6)0.707994 (5)0.01407 (4)
O10.6518 (3)0.57008 (11)0.83910 (10)0.0215 (4)
O20.6004 (3)0.43217 (11)0.77043 (10)0.0221 (4)
O30.3666 (2)0.67625 (11)0.74664 (10)0.0171 (4)
O40.2682 (2)0.52341 (11)0.72411 (10)0.0168 (4)
N10.6651 (3)0.49786 (14)0.87218 (11)0.0167 (4)
N20.6420 (3)0.42654 (14)0.84043 (12)0.0207 (5)
N30.2048 (3)0.65180 (13)0.74731 (10)0.0123 (4)
N40.1479 (3)0.57674 (12)0.73517 (11)0.0139 (4)
N50.4379 (3)0.44824 (13)0.60458 (12)0.0156 (4)
N60.3223 (3)0.61102 (14)0.58176 (11)0.0160 (4)
C10.7119 (4)0.49851 (17)0.94969 (14)0.0189 (5)
C20.6692 (4)0.43069 (17)0.98924 (15)0.0228 (6)
H20.61110.38310.96570.027*
C30.7135 (5)0.43430 (18)1.06373 (16)0.0298 (7)
H30.68770.38821.09170.036*
C40.7955 (5)0.5050 (2)1.09786 (15)0.0355 (8)
H40.82290.50751.14900.043*
C50.8371 (5)0.57181 (19)1.05735 (16)0.0345 (8)
H50.89470.61961.08080.041*
C60.7950 (4)0.56902 (18)0.98277 (15)0.0254 (6)
H60.82250.61470.95480.031*
C70.0758 (3)0.71352 (15)0.75744 (13)0.0132 (5)
C8−0.0737 (3)0.68857 (16)0.78329 (13)0.0159 (5)
H8−0.08650.63250.79800.019*
C9−0.2042 (4)0.74779 (17)0.78711 (14)0.0193 (5)
H9−0.30890.73190.80340.023*
C10−0.1817 (4)0.83009 (17)0.76720 (14)0.0211 (6)
H10−0.27220.87010.76860.025*
C11−0.0270 (4)0.85391 (16)0.74523 (14)0.0187 (5)
H11−0.00990.91080.73380.022*
C120.1030 (3)0.79543 (15)0.73976 (13)0.0156 (5)
H120.20840.81150.72420.019*
C130.4890 (4)0.36929 (17)0.61474 (14)0.0195 (6)
H130.56400.35500.65900.023*
C140.4390 (4)0.30593 (17)0.56419 (14)0.0213 (6)
H140.47860.25020.57430.026*
C150.3320 (4)0.32538 (17)0.49995 (14)0.0202 (6)
H150.29740.28320.46470.024*
C160.2737 (3)0.40803 (17)0.48634 (14)0.0174 (5)
C170.3300 (3)0.46863 (17)0.54094 (13)0.0153 (5)
C180.1582 (4)0.43202 (17)0.42116 (14)0.0204 (6)
H180.12050.39120.38500.024*
C190.1015 (4)0.51195 (18)0.41007 (14)0.0198 (6)
H190.02430.52630.36640.024*
C200.1563 (4)0.57524 (16)0.46329 (14)0.0177 (5)
C210.2698 (3)0.55380 (16)0.52921 (13)0.0156 (5)
C220.0991 (4)0.65833 (18)0.45407 (14)0.0210 (6)
H220.02370.67500.41060.025*
C230.1520 (4)0.71536 (18)0.50770 (14)0.0217 (6)
H230.11360.77180.50210.026*
C240.2643 (3)0.68889 (17)0.57130 (14)0.0194 (5)
H240.30020.72870.60850.023*
U11U22U33U12U13U23
Pb10.01178 (6)0.01599 (6)0.01461 (5)−0.00027 (4)0.00298 (4)−0.00125 (3)
O10.0316 (12)0.0155 (10)0.0164 (9)−0.0056 (8)0.0021 (8)0.0018 (7)
O20.0287 (12)0.0188 (10)0.0172 (9)0.0091 (8)0.0003 (8)−0.0034 (7)
O30.0097 (8)0.0152 (9)0.0267 (9)−0.0040 (7)0.0043 (7)−0.0032 (7)
O40.0155 (9)0.0112 (9)0.0250 (9)0.0015 (7)0.0073 (7)−0.0010 (7)
N10.0163 (11)0.0166 (11)0.0173 (10)0.0003 (9)0.0031 (8)0.0008 (9)
N20.0243 (13)0.0184 (12)0.0181 (11)0.0058 (9)0.0008 (9)−0.0022 (9)
N30.0109 (10)0.0117 (10)0.0137 (9)0.0006 (8)0.0006 (8)0.0003 (8)
N40.0140 (11)0.0102 (10)0.0175 (10)−0.0011 (8)0.0033 (8)0.0001 (8)
N50.0143 (11)0.0172 (11)0.0162 (10)0.0009 (9)0.0049 (9)0.0002 (8)
N60.0139 (11)0.0187 (11)0.0160 (10)0.0012 (9)0.0047 (8)0.0001 (9)
C10.0192 (14)0.0211 (14)0.0157 (12)0.0002 (11)0.0015 (10)0.0006 (10)
C20.0258 (16)0.0186 (14)0.0225 (14)−0.0020 (11)0.0004 (11)0.0013 (11)
C30.043 (2)0.0256 (16)0.0197 (14)−0.0043 (14)0.0019 (13)0.0061 (11)
C40.058 (2)0.0329 (18)0.0131 (13)−0.0125 (16)−0.0011 (13)0.0020 (12)
C50.053 (2)0.0283 (17)0.0179 (14)−0.0126 (15)−0.0028 (14)−0.0020 (12)
C60.0319 (17)0.0239 (16)0.0197 (13)−0.0081 (12)0.0031 (12)0.0041 (11)
C70.0126 (12)0.0131 (12)0.0128 (11)0.0004 (9)−0.0002 (9)−0.0021 (9)
C80.0152 (13)0.0117 (12)0.0204 (12)−0.0026 (10)0.0025 (10)−0.0019 (10)
C90.0158 (13)0.0186 (14)0.0237 (13)−0.0008 (11)0.0041 (11)−0.0066 (10)
C100.0202 (14)0.0175 (13)0.0249 (13)0.0068 (11)0.0023 (11)−0.0047 (11)
C110.0245 (15)0.0108 (12)0.0193 (12)0.0002 (11)0.0007 (11)−0.0009 (10)
C120.0167 (13)0.0130 (12)0.0163 (11)−0.0010 (10)0.0010 (10)−0.0005 (10)
C130.0178 (14)0.0215 (14)0.0202 (13)0.0035 (11)0.0059 (11)−0.0002 (11)
C140.0225 (14)0.0148 (13)0.0288 (14)0.0008 (11)0.0100 (11)−0.0006 (11)
C150.0197 (14)0.0196 (14)0.0230 (13)−0.0040 (11)0.0082 (11)−0.0043 (11)
C160.0140 (13)0.0218 (13)0.0186 (12)−0.0045 (11)0.0085 (10)−0.0022 (10)
C170.0101 (12)0.0196 (13)0.0175 (12)−0.0046 (10)0.0059 (10)−0.0019 (10)
C180.0192 (14)0.0249 (15)0.0180 (12)−0.0082 (11)0.0060 (11)−0.0036 (11)
C190.0163 (13)0.0294 (15)0.0135 (12)−0.0051 (11)0.0020 (10)0.0003 (10)
C200.0145 (13)0.0254 (15)0.0146 (12)−0.0024 (11)0.0062 (10)0.0024 (10)
C210.0127 (13)0.0206 (14)0.0152 (12)−0.0025 (10)0.0068 (10)−0.0008 (10)
C220.0143 (13)0.0293 (15)0.0188 (12)0.0008 (11)0.0018 (10)0.0078 (11)
C230.0207 (14)0.0219 (15)0.0238 (13)0.0004 (11)0.0073 (11)0.0044 (11)
C240.0198 (13)0.0187 (13)0.0212 (12)0.0003 (11)0.0080 (10)−0.0002 (10)
Pb1—O42.3106 (18)C7—C81.392 (3)
Pb1—O22.4270 (18)C8—C91.393 (4)
Pb1—O32.4457 (17)C8—H80.9500
Pb1—O12.4586 (19)C9—C101.389 (4)
Pb1—N52.715 (2)C9—H90.9500
Pb1—N62.763 (2)C10—C111.387 (4)
O1—N11.308 (3)C10—H100.9500
O2—N21.304 (3)C11—C121.389 (4)
O3—N31.309 (3)C11—H110.9500
O4—N41.305 (3)C12—H120.9500
N1—N21.285 (3)C13—C141.396 (4)
N1—C11.440 (3)C13—H130.9500
N3—N41.284 (3)C14—C151.367 (4)
N3—C71.439 (3)C14—H140.9500
N5—C131.326 (3)C15—C161.404 (4)
N5—C171.365 (3)C15—H150.9500
N6—C241.325 (3)C16—C171.422 (4)
N6—C211.354 (3)C16—C181.428 (4)
C1—C61.386 (4)C17—C211.443 (4)
C1—C21.392 (4)C18—C191.354 (4)
C2—C31.385 (4)C18—H180.9500
C2—H20.9500C19—C201.433 (4)
C3—C41.392 (4)C19—H190.9500
C3—H30.9500C20—C221.401 (4)
C4—C51.387 (4)C20—C211.421 (4)
C4—H40.9500C22—C231.367 (4)
C5—C61.385 (4)C22—H220.9500
C5—H50.9500C23—C241.406 (4)
C6—H60.9500C23—H230.9500
C7—C121.378 (3)C24—H240.9500
O4—Pb1—O276.42 (7)C8—C7—N3119.2 (2)
O4—Pb1—O365.37 (6)C7—C8—C9118.5 (2)
O2—Pb1—O3123.25 (6)C7—C8—H8120.8
O4—Pb1—O190.97 (7)C9—C8—H8120.8
O2—Pb1—O162.97 (6)C10—C9—C8120.1 (2)
O3—Pb1—O176.93 (6)C10—C9—H9119.9
O4—Pb1—N574.56 (6)C8—C9—H9119.9
O2—Pb1—N575.51 (6)C11—C10—C9120.0 (2)
O3—Pb1—N5127.08 (6)C11—C10—H10120.0
O1—Pb1—N5138.25 (6)C9—C10—H10120.0
O4—Pb1—N675.59 (6)C10—C11—C12120.7 (2)
O2—Pb1—N6132.52 (7)C10—C11—H11119.7
O3—Pb1—N676.70 (6)C12—C11—H11119.7
O1—Pb1—N6153.50 (7)C7—C12—C11118.5 (2)
N5—Pb1—N660.47 (6)C7—C12—H12120.8
N1—O1—Pb1115.64 (14)C11—C12—H12120.8
N2—O2—Pb1122.70 (14)N5—C13—C14123.8 (3)
N3—O3—Pb1112.12 (13)N5—C13—H13118.1
N4—O4—Pb1122.37 (14)C14—C13—H13118.1
N2—N1—O1124.7 (2)C15—C14—C13118.9 (3)
N2—N1—C1117.8 (2)C15—C14—H14120.5
O1—N1—C1117.5 (2)C13—C14—H14120.5
N1—N2—O2113.4 (2)C14—C15—C16119.7 (2)
N4—N3—O3124.9 (2)C14—C15—H15120.2
N4—N3—C7116.4 (2)C16—C15—H15120.2
O3—N3—C7118.64 (19)C15—C16—C17117.8 (2)
N3—N4—O4114.2 (2)C15—C16—C18122.4 (2)
C13—N5—C17118.0 (2)C17—C16—C18119.8 (3)
C13—N5—Pb1120.57 (17)N5—C17—C16121.8 (2)
C17—N5—Pb1121.42 (16)N5—C17—C21119.0 (2)
C24—N6—C21118.7 (2)C16—C17—C21119.2 (2)
C24—N6—Pb1121.10 (17)C19—C18—C16121.1 (2)
C21—N6—Pb1120.19 (16)C19—C18—H18119.4
C6—C1—C2121.9 (2)C16—C18—H18119.4
C6—C1—N1118.0 (2)C18—C19—C20121.0 (2)
C2—C1—N1120.1 (2)C18—C19—H19119.5
C3—C2—C1118.4 (3)C20—C19—H19119.5
C3—C2—H2120.8C22—C20—C21117.7 (2)
C1—C2—H2120.8C22—C20—C19122.6 (2)
C2—C3—C4120.5 (3)C21—C20—C19119.7 (2)
C2—C3—H3119.8N6—C21—C20121.9 (2)
C4—C3—H3119.8N6—C21—C17118.9 (2)
C5—C4—C3120.2 (3)C20—C21—C17119.3 (2)
C5—C4—H4119.9C23—C22—C20119.9 (3)
C3—C4—H4119.9C23—C22—H22120.0
C6—C5—C4120.1 (3)C20—C22—H22120.0
C6—C5—H5119.9C22—C23—C24118.8 (3)
C4—C5—H5119.9C22—C23—H23120.6
C1—C6—C5119.0 (3)C24—C23—H23120.6
C1—C6—H6120.5N6—C24—C23123.1 (3)
C5—C6—H6120.5N6—C24—H24118.5
C12—C7—C8122.1 (2)C23—C24—H24118.5
C12—C7—N3118.6 (2)
O4—Pb1—O1—N168.29 (18)C1—C2—C3—C41.3 (5)
O2—Pb1—O1—N1−5.91 (16)C2—C3—C4—C5−1.4 (6)
O3—Pb1—O1—N1132.71 (18)C3—C4—C5—C61.0 (6)
N5—Pb1—O1—N10.7 (2)C2—C1—C6—C50.3 (5)
N6—Pb1—O1—N1126.70 (18)N1—C1—C6—C5178.4 (3)
O4—Pb1—O2—N2−92.0 (2)C4—C5—C6—C1−0.4 (5)
O3—Pb1—O2—N2−44.2 (2)N4—N3—C7—C12−152.2 (2)
O1—Pb1—O2—N26.17 (19)O3—N3—C7—C1223.7 (3)
N5—Pb1—O2—N2−169.3 (2)N4—N3—C7—C826.5 (3)
N6—Pb1—O2—N2−147.37 (18)O3—N3—C7—C8−157.6 (2)
O4—Pb1—O3—N3−7.02 (13)C12—C7—C8—C93.9 (4)
O2—Pb1—O3—N3−59.47 (16)N3—C7—C8—C9−174.7 (2)
O1—Pb1—O3—N3−104.23 (15)C7—C8—C9—C10−1.7 (4)
N5—Pb1—O3—N337.44 (17)C8—C9—C10—C11−1.7 (4)
N6—Pb1—O3—N373.02 (14)C9—C10—C11—C122.9 (4)
O2—Pb1—O4—N4146.36 (18)C8—C7—C12—C11−2.7 (4)
O3—Pb1—O4—N49.37 (16)N3—C7—C12—C11176.0 (2)
O1—Pb1—O4—N484.50 (17)C10—C11—C12—C7−0.8 (4)
N5—Pb1—O4—N4−135.20 (18)C17—N5—C13—C140.0 (4)
N6—Pb1—O4—N4−72.39 (17)Pb1—N5—C13—C14179.90 (19)
Pb1—O1—N1—N26.5 (3)N5—C13—C14—C150.5 (4)
Pb1—O1—N1—C1−174.66 (17)C13—C14—C15—C16−0.5 (4)
O1—N1—N2—O2−1.0 (4)C14—C15—C16—C170.2 (4)
C1—N1—N2—O2−179.9 (2)C14—C15—C16—C18−178.3 (2)
Pb1—O2—N2—N1−5.4 (3)C13—N5—C17—C16−0.4 (4)
Pb1—O3—N3—N45.5 (3)Pb1—N5—C17—C16179.72 (17)
Pb1—O3—N3—C7−170.04 (15)C13—N5—C17—C21178.8 (2)
O3—N3—N4—O42.4 (3)Pb1—N5—C17—C21−1.1 (3)
C7—N3—N4—O4177.98 (19)C15—C16—C17—N50.3 (4)
Pb1—O4—N4—N3−10.2 (3)C18—C16—C17—N5178.9 (2)
O4—Pb1—N5—C13−96.9 (2)C15—C16—C17—C21−178.9 (2)
O2—Pb1—N5—C13−17.25 (19)C18—C16—C17—C21−0.3 (4)
O3—Pb1—N5—C13−138.21 (18)C15—C16—C18—C19178.8 (3)
O1—Pb1—N5—C13−23.3 (2)C17—C16—C18—C190.3 (4)
N6—Pb1—N5—C13−178.8 (2)C16—C18—C19—C200.3 (4)
O4—Pb1—N5—C1783.03 (18)C18—C19—C20—C22−179.3 (3)
O2—Pb1—N5—C17162.6 (2)C18—C19—C20—C21−0.9 (4)
O3—Pb1—N5—C1741.7 (2)C24—N6—C21—C200.6 (4)
O1—Pb1—N5—C17156.59 (17)Pb1—N6—C21—C20−179.48 (18)
N6—Pb1—N5—C171.10 (17)C24—N6—C21—C17−178.8 (2)
O4—Pb1—N6—C2498.62 (19)Pb1—N6—C21—C171.0 (3)
O2—Pb1—N6—C24154.25 (17)C22—C20—C21—N6−0.1 (4)
O3—Pb1—N6—C2431.04 (18)C19—C20—C21—N6−178.6 (2)
O1—Pb1—N6—C2437.1 (3)C22—C20—C21—C17179.4 (2)
N5—Pb1—N6—C24178.8 (2)C19—C20—C21—C170.9 (4)
O4—Pb1—N6—C21−81.27 (18)N5—C17—C21—N60.0 (3)
O2—Pb1—N6—C21−25.6 (2)C16—C17—C21—N6179.2 (2)
O3—Pb1—N6—C21−148.84 (19)N5—C17—C21—C20−179.5 (2)
O1—Pb1—N6—C21−142.83 (17)C16—C17—C21—C20−0.3 (4)
N5—Pb1—N6—C21−1.08 (17)C21—C20—C22—C23−0.4 (4)
N2—N1—C1—C6158.2 (3)C19—C20—C22—C23178.1 (2)
O1—N1—C1—C6−20.8 (4)C20—C22—C23—C240.3 (4)
N2—N1—C1—C2−23.7 (4)C21—N6—C24—C23−0.7 (4)
O1—N1—C1—C2157.4 (3)Pb1—N6—C24—C23179.37 (18)
C6—C1—C2—C3−0.7 (5)C22—C23—C24—N60.3 (4)
N1—C1—C2—C3−178.8 (3)
  2 in total

1.  A short history of SHELX.

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

2.  Bis(μ-N-nitroso-N-phenyl-hydroxy-laminato)-κO,O':O';κO':O,O'-bis-[(N-nitroso-N-phenyl-hydroxy-laminato-κO,O')lead(II)].

Authors:  Ezzatollah Najafi; Mostafa M Amini; Seik Weng Ng
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-02-26
  2 in total

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