Download citation
Download citation
link to html
The dinuclear title compound, [Pb2(C6H8O4)(NO3)2(C19H13N5)2], lies with the mid-point of the butyl chain of the bridging adipate unit on a center of inversion. The PbII ion is covalently bonded to the nitrate anion and is bonded to a carboxyl­ate group of the adipate unit by another covalent bond. The N-heterocycle functions in a chelating tridentate mode. The metal atom exists in a Ψ-octa­hedral coordination environment. When weaker Pb...O inter­actions are also considered, the geometry is a Ψ-tricapped trigonal prism in which the lone-pair electrons occupy one face of the trigonal prism. Adjacent mol­ecules are linked into a layer structure by N—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536809052647/bt5131sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536809052647/bt5131Isup2.hkl
Contains datablock I

CCDC reference: 766674

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.012 Å
  • R factor = 0.041
  • wR factor = 0.099
  • Data-to-parameter ratio = 14.9

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for N6
Author Response: This belong to the nitrate ion. There is some possible disorder in the oxygen atoms but it is not necessary to treat it. The ion binds through only one oxygen atom .

Alert level B PLAT220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 4.18 Ratio PLAT152_ALERT_1_B The Supplied and Calc. Volume s.u. Differ by ... 4 Units
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O3 PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 12 PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 34 PLAT971_ALERT_2_C Large Calcd. Non-Metal Positive Residual Density 1.76 eA-3 PLAT971_ALERT_2_C Large Calcd. Non-Metal Positive Residual Density 1.61 eA-3 PLAT971_ALERT_2_C Large Calcd. Non-Metal Positive Residual Density 1.58 eA-3 PLAT971_ALERT_2_C Large Calcd. Non-Metal Positive Residual Density 1.52 eA-3 PLAT041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ? PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 78
Alert level G PLAT154_ALERT_1_G The su's on the Cell Angles are Equal (x 10000) 100 Deg. PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature 293 K
1 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Related literature top

For the structure of Pb2(C6H8O4)2(C19H13N5)2 and lone-pair sterechemistry, see: Meng et al. (2009).

Experimental top

Lead nitrate (0.250 mmol), 2-(6-(1H-benzo[d]imidazol-2-yl)pyridin-2-yl)-1H-benzo[d]imidazole (0.250 mmol), adipic acid (0.125 mmol) and water (10 ml) were sealed in a 25 ml Teflon-lined, stainless-steel Parr bomb. The bomb was heated at 413 K for 4 days and cooled to room temperature. Brown block-shaped crystals were colleacted and washed in water; the yield was 25%.

Refinement top

Hydrogen atoms were generated geometrically and were constrained to ride on their parent atoms [C–H = 0.93, N–H 0.86 Å; Uiso(H) =1.2Ueq(C,N)].

The final difference Fourier map had a peak near C14 and a hole near H2a.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); 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, 2009).

Figures top
[Figure 1] Fig. 1. Anisotropic displacement ellipsoid plot (Barbour, 2001) of Pb2(NO3)2(C6H8O4)(C19H13N5)2 at the 70% probability level; hydrogen atoms are drawn as sphere of arbitrary radius.
[Figure 2] Fig. 2. Detail of the coordination environment of the PbII centre.
µ-Adipato-κ2O1:O4-bis{[2,6-bis(1H-benzimidazol-2- yl-κN3)pyridine-κN](nitrato-κO)lead(II)} top
Crystal data top
[Pb2(C6H8O4)(NO3)2(C19H13N5)2]Z = 1
Mr = 1305.21F(000) = 626
Triclinic, P1Dx = 2.047 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.3470 (7) ÅCell parameters from 3150 reflections
b = 10.6433 (8) Åθ = 2.2–24.8°
c = 11.3776 (8) ŵ = 8.02 mm1
α = 106.696 (1)°T = 293 K
β = 95.343 (1)°Block, brown
γ = 99.117 (1)°0.26 × 0.12 × 0.08 mm
V = 1058.9 (1) Å3
Data collection top
Bruker APEXII
diffractometer
4561 independent reflections
Radiation source: fine-focus sealed tube3586 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
ϕ and ω scansθmax = 27.1°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1111
Tmin = 0.230, Tmax = 0.566k = 1313
8299 measured reflectionsl = 1414
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)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.099H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0524P)2]
where P = (Fo2 + 2Fc2)/3
4561 reflections(Δ/σ)max = 0.001
307 parametersΔρmax = 1.93 e Å3
0 restraintsΔρmin = 1.17 e Å3
Crystal data top
[Pb2(C6H8O4)(NO3)2(C19H13N5)2]γ = 99.117 (1)°
Mr = 1305.21V = 1058.9 (1) Å3
Triclinic, P1Z = 1
a = 9.3470 (7) ÅMo Kα radiation
b = 10.6433 (8) ŵ = 8.02 mm1
c = 11.3776 (8) ÅT = 293 K
α = 106.696 (1)°0.26 × 0.12 × 0.08 mm
β = 95.343 (1)°
Data collection top
Bruker APEXII
diffractometer
4561 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3586 reflections with I > 2σ(I)
Tmin = 0.230, Tmax = 0.566Rint = 0.036
8299 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0410 restraints
wR(F2) = 0.099H-atom parameters constrained
S = 1.02Δρmax = 1.93 e Å3
4561 reflectionsΔρmin = 1.17 e Å3
307 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb11.07669 (3)0.71714 (3)0.65491 (3)0.02682 (11)
O10.8637 (6)0.6980 (5)0.5092 (5)0.0341 (13)
O20.8304 (6)0.4985 (5)0.5330 (5)0.0381 (13)
O31.2560 (7)0.8902 (7)0.8623 (6)0.0579 (18)
O41.3952 (11)0.7543 (10)0.8022 (10)0.126 (5)
O51.4055 (12)0.8554 (14)0.9916 (9)0.141 (5)
N11.1854 (7)0.8782 (6)0.5449 (5)0.0286 (14)
N21.2263 (6)1.0797 (6)0.5237 (5)0.0274 (14)
H21.22151.16210.53430.033*
N31.0091 (7)0.9473 (6)0.7236 (5)0.0251 (13)
N40.8962 (7)0.7470 (6)0.8149 (6)0.0329 (15)
N50.7760 (7)0.8747 (6)0.9451 (6)0.0352 (16)
H50.74350.94400.98390.042*
N61.3504 (9)0.8307 (8)0.8859 (7)0.052 (2)
C11.2754 (8)0.8763 (7)0.4564 (7)0.0262 (16)
C21.3328 (9)0.7741 (8)0.3826 (7)0.0324 (18)
H2A1.31320.68820.38930.039*
C31.4197 (9)0.8036 (8)0.2989 (7)0.0349 (19)
H31.46000.73660.24900.042*
C41.4490 (9)0.9331 (9)0.2873 (7)0.0369 (19)
H41.50850.94990.23030.044*
C51.3918 (8)1.0343 (8)0.3581 (7)0.0350 (19)
H5A1.41061.12000.35080.042*
C61.3046 (8)1.0032 (7)0.4412 (7)0.0278 (16)
C71.1608 (8)1.0009 (7)0.5828 (6)0.0258 (16)
C81.0701 (7)1.0443 (7)0.6764 (6)0.0208 (14)
C91.0481 (8)1.1737 (7)0.7213 (8)0.0344 (18)
H91.08871.23920.68820.041*
C100.9640 (9)1.2052 (8)0.8172 (7)0.038 (2)
H100.95091.29260.84950.045*
C110.9004 (9)1.1077 (8)0.8642 (7)0.0340 (18)
H110.84281.12760.92690.041*
C120.9248 (8)0.9783 (7)0.8148 (7)0.0263 (16)
C130.8642 (8)0.8677 (8)0.8563 (7)0.0299 (17)
C140.7477 (9)0.7502 (8)0.9616 (8)0.0345 (18)
C150.6696 (9)0.7026 (9)1.0431 (8)0.041 (2)
H150.61690.75501.09600.049*
C160.6744 (9)0.5751 (10)1.0410 (8)0.046 (2)
H160.62580.54011.09580.056*
C170.7503 (11)0.4942 (10)0.9588 (9)0.056 (3)
H170.74830.40660.95900.067*
C180.8266 (11)0.5409 (9)0.8793 (9)0.050 (2)
H180.87820.48760.82610.060*
C190.8245 (9)0.6720 (8)0.8805 (7)0.0333 (18)
C200.7885 (8)0.5807 (7)0.4878 (7)0.0264 (16)
C210.6450 (8)0.5467 (8)0.4015 (8)0.039 (2)
H21A0.66060.49890.31870.047*
H21B0.61590.62920.39820.047*
C220.5208 (9)0.4628 (8)0.4384 (7)0.038 (2)
H22A0.55000.38110.44430.045*
H22B0.43610.43830.37460.045*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.02973 (17)0.02289 (16)0.03042 (16)0.00981 (11)0.00830 (11)0.00846 (11)
O10.030 (3)0.025 (3)0.046 (3)0.003 (2)0.003 (3)0.013 (2)
O20.041 (3)0.027 (3)0.051 (4)0.009 (3)0.010 (3)0.016 (3)
O30.053 (4)0.060 (4)0.052 (4)0.031 (4)0.009 (3)0.001 (3)
O40.127 (9)0.126 (9)0.097 (7)0.085 (7)0.009 (6)0.034 (6)
O50.122 (9)0.244 (14)0.055 (6)0.098 (9)0.008 (6)0.017 (7)
N10.035 (4)0.022 (3)0.030 (3)0.007 (3)0.011 (3)0.008 (3)
N20.030 (3)0.022 (3)0.031 (3)0.006 (3)0.007 (3)0.008 (3)
N30.031 (3)0.019 (3)0.025 (3)0.009 (3)0.003 (3)0.004 (2)
N40.038 (4)0.029 (4)0.036 (4)0.011 (3)0.016 (3)0.010 (3)
N50.033 (4)0.033 (4)0.039 (4)0.010 (3)0.019 (3)0.004 (3)
N60.057 (5)0.062 (5)0.037 (4)0.029 (4)0.006 (4)0.005 (4)
C10.022 (4)0.025 (4)0.028 (4)0.002 (3)0.002 (3)0.007 (3)
C20.042 (5)0.027 (4)0.032 (4)0.014 (4)0.011 (4)0.010 (3)
C30.036 (5)0.042 (5)0.027 (4)0.014 (4)0.010 (3)0.006 (3)
C40.036 (5)0.050 (5)0.027 (4)0.007 (4)0.007 (4)0.015 (4)
C50.033 (4)0.033 (4)0.040 (5)0.003 (4)0.002 (4)0.019 (4)
C60.022 (4)0.030 (4)0.028 (4)0.004 (3)0.000 (3)0.005 (3)
C70.025 (4)0.024 (4)0.024 (4)0.000 (3)0.001 (3)0.004 (3)
C80.009 (3)0.027 (4)0.020 (3)0.002 (3)0.007 (3)0.002 (3)
C90.032 (4)0.022 (4)0.045 (5)0.000 (3)0.005 (4)0.012 (3)
C100.050 (5)0.023 (4)0.039 (5)0.018 (4)0.011 (4)0.001 (3)
C110.034 (4)0.034 (4)0.031 (4)0.009 (4)0.013 (3)0.001 (3)
C120.029 (4)0.019 (4)0.030 (4)0.010 (3)0.003 (3)0.003 (3)
C130.028 (4)0.029 (4)0.029 (4)0.005 (3)0.002 (3)0.005 (3)
C140.034 (5)0.027 (4)0.042 (5)0.004 (3)0.005 (4)0.011 (4)
C150.027 (4)0.049 (5)0.048 (5)0.003 (4)0.018 (4)0.015 (4)
C160.038 (5)0.060 (6)0.047 (5)0.003 (4)0.012 (4)0.029 (5)
C170.068 (7)0.047 (6)0.046 (6)0.006 (5)0.008 (5)0.013 (5)
C180.070 (7)0.032 (5)0.054 (6)0.016 (5)0.027 (5)0.014 (4)
C190.033 (4)0.032 (4)0.035 (4)0.009 (4)0.012 (4)0.007 (3)
C200.026 (4)0.019 (4)0.031 (4)0.003 (3)0.012 (3)0.002 (3)
C210.036 (5)0.036 (5)0.041 (5)0.005 (4)0.004 (4)0.012 (4)
C220.032 (4)0.035 (5)0.036 (5)0.000 (4)0.006 (4)0.001 (4)
Geometric parameters (Å, º) top
Pb1—O12.411 (5)C4—C51.364 (11)
Pb1—N12.541 (6)C4—H40.9300
Pb1—N32.548 (6)C5—C61.380 (11)
Pb1—N42.583 (6)C5—H5A0.9300
Pb1—O32.749 (6)C7—C81.441 (10)
Pb1—O22.914 (6)C8—C91.381 (10)
Pb1—O2i2.958 (5)C9—C101.397 (11)
Pb1—O43.185 (10)C9—H90.9300
O1—C201.275 (9)C10—C111.378 (11)
O2—C201.231 (9)C10—H100.9300
O3—N61.217 (9)C11—C121.393 (10)
O4—N61.216 (11)C11—H110.9300
O5—N61.200 (11)C12—C131.445 (11)
N1—C71.317 (9)C14—C151.389 (11)
N1—C11.369 (9)C14—C191.389 (11)
N2—C71.330 (9)C15—C161.359 (12)
N2—C61.399 (9)C15—H150.9300
N2—H20.8600C16—C171.405 (13)
N3—C121.358 (9)C16—H160.9300
N3—C81.367 (9)C17—C181.356 (13)
N4—C131.327 (9)C17—H170.9300
N4—C191.382 (10)C18—C191.394 (12)
N5—C131.356 (9)C18—H180.9300
N5—C141.379 (10)C20—C211.513 (11)
N5—H50.8600C21—C221.516 (11)
C1—C21.386 (10)C21—H21A0.9700
C1—C61.399 (10)C21—H21B0.9700
C2—C31.378 (11)C22—C22ii1.519 (14)
C2—H2A0.9300C22—H22A0.9700
C3—C41.408 (11)C22—H22B0.9700
C3—H30.9300
O1—Pb1—N181.15 (19)C3—C4—H4119.3
O1—Pb1—N376.12 (18)C4—C5—C6116.6 (7)
N1—Pb1—N365.32 (19)C4—C5—H5A121.7
O1—Pb1—N483.9 (2)C6—C5—H5A121.7
N1—Pb1—N4129.70 (19)C5—C6—C1123.5 (7)
N3—Pb1—N464.51 (19)C5—C6—N2131.7 (7)
O1—Pb1—O3142.75 (18)C1—C6—N2104.8 (6)
N1—Pb1—O384.8 (2)N1—C7—N2112.8 (6)
N3—Pb1—O366.66 (19)N1—C7—C8123.6 (7)
N4—Pb1—O378.9 (2)N2—C7—C8123.6 (7)
O1—Pb1—O247.51 (16)N3—C8—C9120.6 (6)
N1—Pb1—O2121.65 (18)N3—C8—C7114.8 (6)
N3—Pb1—O2114.54 (17)C9—C8—C7124.5 (7)
N4—Pb1—O277.49 (18)C8—C9—C10119.2 (7)
O3—Pb1—O2152.3 (2)C8—C9—H9120.4
O1—Pb1—O2i89.14 (17)C10—C9—H9120.4
N1—Pb1—O2i87.79 (17)C11—C10—C9120.6 (7)
N3—Pb1—O2i150.76 (17)C11—C10—H10119.7
N4—Pb1—O2i139.77 (18)C9—C10—H10119.7
O3—Pb1—O2i124.72 (17)C10—C11—C12118.0 (7)
O2—Pb1—O2i68.94 (18)C10—C11—H11121.0
O1—Pb1—O4167.8 (3)C12—C11—H11121.0
N1—Pb1—O488.3 (3)N3—C12—C11121.9 (7)
N3—Pb1—O4105.0 (2)N3—C12—C13114.9 (6)
N4—Pb1—O4107.6 (2)C11—C12—C13123.2 (7)
O3—Pb1—O440.80 (19)N4—C13—N5111.9 (7)
O2—Pb1—O4137.4 (2)N4—C13—C12122.8 (7)
O2i—Pb1—O484.36 (19)N5—C13—C12125.2 (7)
C20—O1—Pb1106.6 (5)N5—C14—C15131.9 (8)
C20—O2—Pb183.5 (4)N5—C14—C19105.6 (7)
N6—O3—Pb1105.7 (5)C15—C14—C19122.4 (8)
N6—O4—Pb184.3 (6)C16—C15—C14116.2 (8)
C7—N1—C1106.2 (6)C16—C15—H15121.9
C7—N1—Pb1116.8 (4)C14—C15—H15121.9
C1—N1—Pb1136.9 (5)C15—C16—C17122.1 (8)
C7—N2—C6107.1 (6)C15—C16—H16118.9
C7—N2—H2126.5C17—C16—H16118.9
C6—N2—H2126.5C18—C17—C16121.6 (9)
C12—N3—C8119.6 (6)C18—C17—H17119.2
C12—N3—Pb1120.8 (5)C16—C17—H17119.2
C8—N3—Pb1119.3 (4)C17—C18—C19117.3 (9)
C13—N4—C19105.6 (6)C17—C18—H18121.3
C13—N4—Pb1116.7 (5)C19—C18—H18121.3
C19—N4—Pb1137.6 (5)N4—C19—C14109.5 (7)
C13—N5—C14107.4 (6)N4—C19—C18130.0 (7)
C13—N5—H5126.3C14—C19—C18120.4 (8)
C14—N5—H5126.3O2—C20—O1122.3 (7)
O5—N6—O4120.5 (10)O2—C20—C21121.4 (7)
O5—N6—O3119.2 (9)O1—C20—C21116.4 (7)
O4—N6—O3120.1 (9)C20—C21—C22114.5 (7)
N1—C1—C2131.7 (7)C20—C21—H21A108.6
N1—C1—C6109.1 (6)C22—C21—H21A108.6
C2—C1—C6119.2 (7)C20—C21—H21B108.6
C3—C2—C1118.0 (8)C22—C21—H21B108.6
C3—C2—H2A121.0H21A—C21—H21B107.6
C1—C2—H2A121.0C21—C22—C22ii111.7 (8)
C2—C3—C4121.4 (7)C21—C22—H22A109.3
C2—C3—H3119.3C22ii—C22—H22A109.3
C4—C3—H3119.3C21—C22—H22B109.3
C5—C4—C3121.3 (7)C22ii—C22—H22B109.3
C5—C4—H4119.3H22A—C22—H22B107.9
N1—Pb1—O1—C20151.2 (5)Pb1—N1—C1—C27.0 (13)
N3—Pb1—O1—C20142.2 (5)C7—N1—C1—C60.2 (8)
N4—Pb1—O1—C2077.0 (5)Pb1—N1—C1—C6175.5 (5)
O3—Pb1—O1—C20139.6 (5)N1—C1—C2—C3178.9 (8)
O2—Pb1—O1—C201.6 (4)C6—C1—C2—C31.6 (11)
O2i—Pb1—O1—C2063.3 (5)C1—C2—C3—C40.5 (12)
O4—Pb1—O1—C20120.9 (10)C2—C3—C4—C50.3 (13)
O1—Pb1—O2—C201.6 (4)C3—C4—C5—C60.1 (12)
N1—Pb1—O2—C2037.5 (5)C4—C5—C6—C11.0 (12)
N3—Pb1—O2—C2037.6 (5)C4—C5—C6—N2177.8 (8)
N4—Pb1—O2—C2091.7 (4)N1—C1—C6—C5179.8 (7)
O3—Pb1—O2—C20123.7 (5)C2—C1—C6—C51.9 (12)
O2i—Pb1—O2—C20110.9 (5)N1—C1—C6—N20.7 (8)
O4—Pb1—O2—C20165.8 (4)C2—C1—C6—N2177.2 (7)
O1—Pb1—O3—N6178.2 (5)C7—N2—C6—C5179.7 (8)
N1—Pb1—O3—N6110.1 (6)C7—N2—C6—C11.3 (8)
N3—Pb1—O3—N6175.4 (7)C1—N1—C7—N21.1 (9)
N4—Pb1—O3—N6117.7 (6)Pb1—N1—C7—N2177.5 (5)
O2—Pb1—O3—N685.9 (7)C1—N1—C7—C8179.9 (7)
O2i—Pb1—O3—N626.4 (7)Pb1—N1—C7—C83.7 (9)
O4—Pb1—O3—N616.7 (6)C6—N2—C7—N11.6 (9)
O1—Pb1—O4—N6130.1 (9)C6—N2—C7—C8179.7 (6)
N1—Pb1—O4—N6100.2 (8)C12—N3—C8—C90.7 (10)
N3—Pb1—O4—N636.4 (8)Pb1—N3—C8—C9173.1 (5)
N4—Pb1—O4—N631.1 (8)C12—N3—C8—C7178.2 (6)
O3—Pb1—O4—N616.2 (6)Pb1—N3—C8—C74.4 (8)
O2—Pb1—O4—N6121.7 (7)N1—C7—C8—N30.4 (10)
O2i—Pb1—O4—N6171.8 (8)N2—C7—C8—N3178.2 (6)
O1—Pb1—N1—C782.8 (5)N1—C7—C8—C9177.0 (7)
N3—Pb1—N1—C74.0 (5)N2—C7—C8—C94.4 (11)
N4—Pb1—N1—C78.3 (6)N3—C8—C9—C100.8 (11)
O3—Pb1—N1—C762.6 (5)C7—C8—C9—C10176.4 (7)
O2—Pb1—N1—C7108.7 (5)C8—C9—C10—C111.8 (12)
O2i—Pb1—N1—C7172.2 (5)C9—C10—C11—C121.2 (12)
O4—Pb1—N1—C7103.4 (5)C8—N3—C12—C111.3 (11)
O1—Pb1—N1—C1102.3 (7)Pb1—N3—C12—C11172.4 (6)
N3—Pb1—N1—C1179.0 (8)C8—N3—C12—C13179.1 (6)
N4—Pb1—N1—C1176.8 (6)Pb1—N3—C12—C137.3 (9)
O3—Pb1—N1—C1112.3 (7)C10—C11—C12—N30.4 (12)
O2—Pb1—N1—C176.3 (7)C10—C11—C12—C13180.0 (8)
O2i—Pb1—N1—C112.8 (7)C19—N4—C13—N50.0 (9)
O4—Pb1—N1—C171.6 (7)Pb1—N4—C13—N5176.3 (5)
O1—Pb1—N3—C1295.3 (6)C19—N4—C13—C12176.8 (7)
N1—Pb1—N3—C12178.2 (6)Pb1—N4—C13—C120.5 (10)
N4—Pb1—N3—C125.5 (5)C14—N5—C13—N40.6 (9)
O3—Pb1—N3—C1283.0 (6)C14—N5—C13—C12177.2 (7)
O2—Pb1—N3—C1266.7 (6)N3—C12—C13—N44.4 (11)
O2i—Pb1—N3—C12157.1 (5)C11—C12—C13—N4175.2 (8)
O4—Pb1—N3—C1297.2 (6)N3—C12—C13—N5179.3 (7)
O1—Pb1—N3—C891.0 (5)C11—C12—C13—N51.1 (12)
N1—Pb1—N3—C84.5 (5)C13—N5—C14—C15177.1 (9)
N4—Pb1—N3—C8179.2 (5)C13—N5—C14—C190.8 (9)
O3—Pb1—N3—C890.7 (5)N5—C14—C15—C16174.5 (9)
O2—Pb1—N3—C8119.6 (5)C19—C14—C15—C161.2 (13)
O2i—Pb1—N3—C829.2 (7)C14—C15—C16—C171.8 (14)
O4—Pb1—N3—C876.5 (5)C15—C16—C17—C181.9 (16)
O1—Pb1—N4—C1380.3 (6)C16—C17—C18—C191.2 (16)
N1—Pb1—N4—C137.2 (7)C13—N4—C19—C140.5 (9)
N3—Pb1—N4—C132.9 (5)Pb1—N4—C19—C14175.6 (6)
O3—Pb1—N4—C1366.4 (6)C13—N4—C19—C18176.0 (9)
O2—Pb1—N4—C13128.1 (6)Pb1—N4—C19—C180.9 (15)
O2i—Pb1—N4—C13161.8 (5)N5—C14—C19—N40.8 (9)
O4—Pb1—N4—C1395.7 (6)C15—C14—C19—N4177.5 (8)
O1—Pb1—N4—C19104.9 (8)N5—C14—C19—C18176.1 (8)
N1—Pb1—N4—C19178.1 (7)C15—C14—C19—C180.6 (13)
N3—Pb1—N4—C19177.6 (9)C17—C18—C19—N4176.8 (9)
O3—Pb1—N4—C19108.3 (8)C17—C18—C19—C140.6 (14)
O2—Pb1—N4—C1957.2 (8)Pb1—O2—C20—O12.6 (7)
O2i—Pb1—N4—C1923.5 (9)Pb1—O2—C20—C21178.5 (7)
O4—Pb1—N4—C1979.0 (8)Pb1—O1—C20—O23.2 (8)
Pb1—O4—N6—O5156.9 (12)Pb1—O1—C20—C21177.8 (5)
Pb1—O4—N6—O328.4 (10)O2—C20—C21—C2239.6 (10)
Pb1—O3—N6—O5150.5 (10)O1—C20—C21—C22141.5 (7)
Pb1—O3—N6—O434.7 (12)C20—C21—C22—C22ii64.3 (12)
C7—N1—C1—C2177.7 (8)
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O1iii0.861.952.744 (8)152
N5—H5···O3iv0.862.102.891 (9)153
Symmetry codes: (iii) x+2, y+2, z+1; (iv) x+2, y+2, z+2.

Experimental details

Crystal data
Chemical formula[Pb2(C6H8O4)(NO3)2(C19H13N5)2]
Mr1305.21
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)9.3470 (7), 10.6433 (8), 11.3776 (8)
α, β, γ (°)106.696 (1), 95.343 (1), 99.117 (1)
V3)1058.9 (1)
Z1
Radiation typeMo Kα
µ (mm1)8.02
Crystal size (mm)0.26 × 0.12 × 0.08
Data collection
DiffractometerBruker APEXII
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.230, 0.566
No. of measured, independent and
observed [I > 2σ(I)] reflections
8299, 4561, 3586
Rint0.036
(sin θ/λ)max1)0.641
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.099, 1.02
No. of reflections4561
No. of parameters307
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.93, 1.17

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2009).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O1i0.861.952.744 (8)152
N5—H5···O3ii0.862.102.891 (9)153
Symmetry codes: (i) x+2, y+2, z+1; (ii) x+2, y+2, z+2.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds