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The asymmetric unit of the title compound, (C
4H
12N
2)[Pb(C
7H
3NO
4)
2]·2H
2O, contains two half-cations, one anion and two water molecules. There is a centre of symmetry at the centre of each cation ring. The Pb
II atom is six-coordinated by four O atoms and two N atoms of two tridentate pyridine-2,6-dicarboxylic acid molecules. Intermolecular N—H
O and O—H
O hydrogen bonds and π–π stacking interactions seem to be effective in the stabilization of the crystal structure, resulting in the formation of a three-dimensional network.
Supporting information
CCDC reference: 609298
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean (C-C) = 0.003 Å
- R factor = 0.017
- wR factor = 0.040
- Data-to-parameter ratio = 18.3
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.67
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.07
PLAT411_ALERT_2_C Short Inter H...H Contact H9A .. H9A .. 2.13 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 16
Alert level G
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 0.669
Tmax scaled 0.195 Tmin scaled 0.116
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1998); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL(Sheldrick, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Piperazinediium bis(pyridine-2,6-dicarboxylato)lead(II) dihydrate
top
Crystal data top
(C4H12N2)[Pb(C7H3NO4)2]·2H2O | Z = 2 |
Mr = 661.59 | F(000) = 640 |
Triclinic, P1 | Dx = 2.114 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.3115 (4) Å | Cell parameters from 9297 reflections |
b = 12.5123 (6) Å | θ = 3.0–29.0° |
c = 13.0501 (7) Å | µ = 8.18 mm−1 |
α = 112.670 (1)° | T = 120 K |
β = 102.781 (1)° | Prism, colorless |
γ = 98.162 (1)° | 0.30 × 0.20 × 0.20 mm |
V = 1039.52 (9) Å3 | |
Data collection top
Bruker SMART 1000 CCD area-detector diffractometer | 5457 independent reflections |
Radiation source: normal-focus sealed tube | 5195 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
ω scans | θmax = 29.0°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1998) | h = −9→9 |
Tmin = 0.173, Tmax = 0.291 | k = −17→17 |
11465 measured reflections | l = −17→17 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.017 | Hydrogen site location: geom and difmap |
wR(F2) = 0.040 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0174P)2 + 0.6846P] where P = (Fo2 + 2Fc2)/3 |
5457 reflections | (Δ/σ)max = 0.004 |
298 parameters | Δρmax = 1.73 e Å−3 |
0 restraints | Δρmin = −0.84 e Å−3 |
Special details top
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 | x | y | z | Uiso*/Ueq | |
Pb1 | 0.061636 (11) | 0.771312 (7) | 0.239940 (6) | 0.01045 (3) | |
O1 | −0.0933 (2) | 0.59325 (14) | 0.24451 (14) | 0.0160 (3) | |
O2 | −0.2586 (3) | 0.40184 (15) | 0.15729 (14) | 0.0184 (3) | |
O3 | 0.0375 (2) | 0.81236 (14) | 0.04571 (14) | 0.0142 (3) | |
O4 | −0.1465 (3) | 0.76298 (15) | −0.13491 (15) | 0.0175 (3) | |
O5 | −0.2376 (2) | 0.83044 (15) | 0.20528 (14) | 0.0141 (3) | |
O6 | −0.4712 (2) | 0.90529 (16) | 0.26981 (15) | 0.0174 (3) | |
O7 | 0.2672 (2) | 0.76700 (17) | 0.43353 (15) | 0.0194 (3) | |
O8 | 0.2782 (2) | 0.78039 (15) | 0.61085 (15) | 0.0177 (3) | |
N1 | −0.1490 (3) | 0.60655 (16) | 0.04047 (16) | 0.0105 (3) | |
N2 | −0.0638 (3) | 0.83914 (16) | 0.41305 (15) | 0.0099 (3) | |
C1 | −0.2294 (3) | 0.50242 (19) | 0.03809 (18) | 0.0101 (4) | |
C2 | −0.3438 (3) | 0.4051 (2) | −0.0647 (2) | 0.0143 (4) | |
H2A | −0.3972 | 0.3313 | −0.0646 | 0.017* | |
C3 | −0.3779 (3) | 0.4188 (2) | −0.1673 (2) | 0.0152 (4) | |
H3A | −0.4553 | 0.3540 | −0.2390 | 0.018* | |
C4 | −0.2979 (3) | 0.5281 (2) | −0.16455 (19) | 0.0143 (4) | |
H4A | −0.3217 | 0.5395 | −0.2337 | 0.017* | |
C5 | −0.1828 (3) | 0.62008 (19) | −0.05870 (19) | 0.0108 (4) | |
C6 | −0.1909 (3) | 0.4980 (2) | 0.15510 (19) | 0.0124 (4) | |
C7 | −0.0889 (3) | 0.74192 (19) | −0.04833 (19) | 0.0106 (4) | |
C8 | −0.2311 (3) | 0.87124 (18) | 0.40011 (18) | 0.0097 (4) | |
C9 | −0.3182 (3) | 0.9039 (2) | 0.4881 (2) | 0.0148 (4) | |
H9A | −0.4378 | 0.9256 | 0.4764 | 0.018* | |
C10 | −0.2276 (4) | 0.9043 (2) | 0.5929 (2) | 0.0169 (4) | |
H10A | −0.2831 | 0.9272 | 0.6550 | 0.020* | |
C11 | −0.0534 (3) | 0.8704 (2) | 0.60661 (19) | 0.0156 (4) | |
H11A | 0.0114 | 0.8698 | 0.6779 | 0.019* | |
C12 | 0.0238 (3) | 0.83771 (19) | 0.51402 (19) | 0.0115 (4) | |
C13 | −0.3206 (3) | 0.86881 (19) | 0.28280 (19) | 0.0120 (4) | |
C14 | 0.2065 (3) | 0.7924 (2) | 0.5194 (2) | 0.0133 (4) | |
N1S | 0.8684 (3) | 0.43374 (17) | 0.38381 (16) | 0.0133 (4) | |
H1NA | 0.8213 | 0.4254 | 0.3117 | 0.016* | |
H1NB | 0.8156 | 0.3632 | 0.3835 | 0.016* | |
C1S | 1.0821 (3) | 0.4508 (2) | 0.4065 (2) | 0.0154 (4) | |
H1SB | 1.1369 | 0.5227 | 0.3977 | 0.018* | |
H1SC | 1.1087 | 0.3808 | 0.3485 | 0.018* | |
C2S | 0.8212 (3) | 0.5347 (2) | 0.4720 (2) | 0.0156 (4) | |
H2SA | 0.6790 | 0.5189 | 0.4572 | 0.019* | |
H2SB | 0.8662 | 0.6096 | 0.4656 | 0.019* | |
N2S | 0.5637 (3) | 0.97841 (18) | 0.10009 (17) | 0.0141 (4) | |
H2NA | 0.5409 | 0.9577 | 0.1528 | 0.017* | |
H2NB | 0.6844 | 1.0006 | 0.1178 | 0.017* | |
C3S | 0.4725 (3) | 0.8766 (2) | −0.0170 (2) | 0.0155 (4) | |
H3SA | 0.3313 | 0.8515 | −0.0306 | 0.019* | |
H3SB | 0.5276 | 0.8078 | −0.0211 | 0.019* | |
C4S | 0.4911 (4) | 1.0859 (2) | 0.1097 (2) | 0.0167 (4) | |
H4SA | 0.5578 | 1.1523 | 0.1878 | 0.020* | |
H4SB | 0.3504 | 1.0678 | 0.1002 | 0.020* | |
O1W | 0.9462 (2) | 1.03006 (14) | 0.12047 (14) | 0.0160 (3) | |
H1WA | 1.0012 | 1.0889 | 0.1143 | 0.019* | |
H1WB | 0.9815 | 0.9782 | 0.0951 | 0.019* | |
O2W | 0.5754 (3) | 0.66636 (17) | 0.64453 (16) | 0.0241 (4) | |
H2WA | 0.5126 | 0.7115 | 0.6282 | 0.029* | |
H2WB | 0.6416 | 0.7064 | 0.7131 | 0.029* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pb1 | 0.01146 (4) | 0.01061 (4) | 0.00953 (4) | 0.00207 (3) | 0.00291 (3) | 0.00500 (3) |
O1 | 0.0228 (8) | 0.0119 (8) | 0.0113 (7) | −0.0009 (6) | 0.0032 (6) | 0.0059 (6) |
O2 | 0.0263 (9) | 0.0130 (8) | 0.0143 (8) | −0.0014 (7) | 0.0031 (7) | 0.0081 (7) |
O3 | 0.0171 (8) | 0.0123 (7) | 0.0115 (7) | 0.0003 (6) | 0.0031 (6) | 0.0052 (6) |
O4 | 0.0223 (8) | 0.0143 (8) | 0.0154 (8) | 0.0008 (7) | 0.0006 (7) | 0.0100 (7) |
O5 | 0.0160 (8) | 0.0165 (8) | 0.0113 (7) | 0.0064 (6) | 0.0032 (6) | 0.0072 (6) |
O6 | 0.0140 (8) | 0.0254 (9) | 0.0215 (8) | 0.0091 (7) | 0.0071 (7) | 0.0165 (7) |
O7 | 0.0142 (8) | 0.0287 (10) | 0.0183 (8) | 0.0073 (7) | 0.0040 (7) | 0.0131 (7) |
O8 | 0.0175 (8) | 0.0186 (8) | 0.0159 (8) | 0.0015 (6) | −0.0022 (6) | 0.0113 (7) |
N1 | 0.0113 (8) | 0.0093 (8) | 0.0123 (8) | 0.0046 (7) | 0.0041 (7) | 0.0052 (7) |
N2 | 0.0113 (8) | 0.0079 (8) | 0.0083 (8) | 0.0001 (6) | 0.0008 (6) | 0.0032 (7) |
C1 | 0.0106 (9) | 0.0103 (9) | 0.0116 (9) | 0.0043 (8) | 0.0047 (8) | 0.0055 (8) |
C2 | 0.0161 (10) | 0.0103 (10) | 0.0161 (10) | 0.0017 (8) | 0.0038 (8) | 0.0063 (8) |
C3 | 0.0171 (11) | 0.0122 (10) | 0.0123 (10) | 0.0004 (8) | 0.0017 (8) | 0.0037 (8) |
C4 | 0.0172 (11) | 0.0149 (11) | 0.0120 (10) | 0.0033 (8) | 0.0039 (8) | 0.0076 (9) |
C5 | 0.0117 (9) | 0.0108 (10) | 0.0120 (10) | 0.0046 (8) | 0.0054 (8) | 0.0056 (8) |
C6 | 0.0145 (10) | 0.0120 (10) | 0.0129 (10) | 0.0044 (8) | 0.0054 (8) | 0.0066 (8) |
C7 | 0.0129 (10) | 0.0103 (9) | 0.0118 (9) | 0.0044 (8) | 0.0066 (8) | 0.0059 (8) |
C8 | 0.0121 (9) | 0.0059 (9) | 0.0101 (9) | 0.0007 (7) | 0.0024 (7) | 0.0035 (8) |
C9 | 0.0153 (10) | 0.0120 (10) | 0.0189 (11) | 0.0037 (8) | 0.0074 (9) | 0.0070 (9) |
C10 | 0.0233 (12) | 0.0139 (11) | 0.0148 (11) | 0.0030 (9) | 0.0111 (9) | 0.0051 (9) |
C11 | 0.0217 (11) | 0.0125 (10) | 0.0090 (10) | −0.0002 (9) | 0.0018 (8) | 0.0040 (8) |
C12 | 0.0134 (10) | 0.0072 (9) | 0.0110 (10) | −0.0020 (8) | −0.0001 (8) | 0.0047 (8) |
C13 | 0.0133 (10) | 0.0089 (9) | 0.0136 (10) | 0.0016 (8) | 0.0015 (8) | 0.0066 (8) |
C14 | 0.0114 (10) | 0.0108 (10) | 0.0134 (10) | −0.0020 (8) | −0.0030 (8) | 0.0061 (8) |
N1S | 0.0151 (9) | 0.0132 (9) | 0.0101 (9) | 0.0001 (7) | 0.0019 (7) | 0.0057 (7) |
C1S | 0.0149 (10) | 0.0178 (11) | 0.0140 (10) | 0.0038 (9) | 0.0066 (8) | 0.0062 (9) |
C2S | 0.0135 (10) | 0.0153 (11) | 0.0181 (11) | 0.0033 (8) | 0.0035 (8) | 0.0081 (9) |
N2S | 0.0129 (9) | 0.0197 (10) | 0.0146 (9) | 0.0060 (7) | 0.0047 (7) | 0.0113 (8) |
C3S | 0.0143 (10) | 0.0105 (10) | 0.0219 (11) | 0.0027 (8) | 0.0044 (9) | 0.0079 (9) |
C4S | 0.0197 (11) | 0.0173 (11) | 0.0128 (10) | 0.0083 (9) | 0.0051 (9) | 0.0046 (9) |
O1W | 0.0187 (8) | 0.0107 (7) | 0.0191 (8) | 0.0018 (6) | 0.0103 (7) | 0.0052 (6) |
O2W | 0.0186 (9) | 0.0238 (9) | 0.0227 (9) | 0.0074 (7) | −0.0004 (7) | 0.0057 (8) |
Geometric parameters (Å, º) top
Pb1—O1 | 2.3805 (16) | C9—H9A | 0.9500 |
Pb1—O5 | 2.4123 (16) | C10—C11 | 1.394 (3) |
Pb1—N2 | 2.5150 (18) | C10—H10A | 0.9500 |
Pb1—N1 | 2.5664 (18) | C11—C12 | 1.390 (3) |
Pb1—O7 | 2.6632 (17) | C11—H11A | 0.9500 |
Pb1—O3 | 2.7480 (16) | C12—C14 | 1.522 (3) |
O1—C6 | 1.269 (3) | N1S—C2S | 1.490 (3) |
O2—C6 | 1.248 (3) | N1S—C1S | 1.492 (3) |
O3—C7 | 1.253 (3) | N1S—H1NA | 0.8864 |
O4—C7 | 1.255 (3) | N1S—H1NB | 0.9100 |
O5—C13 | 1.266 (3) | C1S—C2Si | 1.514 (3) |
O6—C13 | 1.253 (3) | C1S—H1SB | 0.9900 |
O7—C14 | 1.241 (3) | C1S—H1SC | 0.9900 |
O8—C14 | 1.267 (3) | C2S—C1Si | 1.514 (3) |
N1—C1 | 1.337 (3) | C2S—H2SA | 0.9900 |
N1—C5 | 1.343 (3) | C2S—H2SB | 0.9900 |
N2—C8 | 1.336 (3) | N2S—C4S | 1.486 (3) |
N2—C12 | 1.340 (3) | N2S—C3S | 1.486 (3) |
C1—C2 | 1.392 (3) | N2S—H2NA | 0.8622 |
C1—C6 | 1.514 (3) | N2S—H2NB | 0.8361 |
C2—C3 | 1.388 (3) | C3S—C4Sii | 1.516 (3) |
C2—H2A | 0.9500 | C3S—H3SA | 0.9900 |
C3—C4 | 1.393 (3) | C3S—H3SB | 0.9900 |
C3—H3A | 0.9500 | C4S—C3Sii | 1.516 (3) |
C4—C5 | 1.388 (3) | C4S—H4SA | 0.9900 |
C4—H4A | 0.9500 | C4S—H4SB | 0.9900 |
C5—C7 | 1.522 (3) | O1W—H1WA | 0.8281 |
C8—C9 | 1.388 (3) | O1W—H1WB | 0.7189 |
C8—C13 | 1.513 (3) | O2W—H2WA | 0.8360 |
C9—C10 | 1.380 (3) | O2W—H2WB | 0.8240 |
| | | |
O1—Pb1—O5 | 92.58 (6) | C9—C10—H10A | 120.4 |
O1—Pb1—N2 | 74.22 (6) | C11—C10—H10A | 120.4 |
O5—Pb1—N2 | 65.89 (5) | C12—C11—C10 | 118.8 (2) |
O1—Pb1—N1 | 65.39 (6) | C12—C11—H11A | 120.6 |
O5—Pb1—N1 | 75.86 (5) | C10—C11—H11A | 120.6 |
N2—Pb1—N1 | 121.92 (6) | N2—C12—C11 | 121.7 (2) |
O1—Pb1—O7 | 73.33 (5) | N2—C12—C14 | 116.3 (2) |
O5—Pb1—O7 | 128.53 (5) | C11—C12—C14 | 122.0 (2) |
N2—Pb1—O7 | 62.65 (6) | O6—C13—O5 | 124.9 (2) |
N1—Pb1—O7 | 133.13 (6) | O6—C13—C8 | 117.5 (2) |
O1—Pb1—O3 | 126.49 (5) | O5—C13—C8 | 117.63 (19) |
O5—Pb1—O3 | 75.51 (5) | O7—C14—O8 | 126.3 (2) |
N2—Pb1—O3 | 137.37 (5) | O7—C14—C12 | 117.72 (19) |
N1—Pb1—O3 | 61.10 (5) | O8—C14—C12 | 115.9 (2) |
O7—Pb1—O3 | 151.30 (5) | C2S—N1S—C1S | 111.46 (17) |
C6—O1—Pb1 | 124.70 (14) | C2S—N1S—H1NA | 113.2 |
C7—O3—Pb1 | 119.24 (13) | C1S—N1S—H1NA | 106.1 |
C13—O5—Pb1 | 122.99 (13) | C2S—N1S—H1NB | 110.2 |
C14—O7—Pb1 | 120.27 (14) | C1S—N1S—H1NB | 109.7 |
C1—N1—C5 | 119.52 (19) | H1NA—N1S—H1NB | 106.0 |
C1—N1—Pb1 | 116.56 (14) | N1S—C1S—C2Si | 110.88 (18) |
C5—N1—Pb1 | 123.91 (14) | N1S—C1S—H1SB | 109.5 |
C8—N2—C12 | 119.34 (19) | C2Si—C1S—H1SB | 109.5 |
C8—N2—Pb1 | 117.72 (13) | N1S—C1S—H1SC | 109.5 |
C12—N2—Pb1 | 122.83 (15) | C2Si—C1S—H1SC | 109.5 |
N1—C1—C2 | 122.3 (2) | H1SB—C1S—H1SC | 108.1 |
N1—C1—C6 | 115.56 (18) | N1S—C2S—C1Si | 110.29 (18) |
C2—C1—C6 | 122.10 (19) | N1S—C2S—H2SA | 109.6 |
C3—C2—C1 | 118.2 (2) | C1Si—C2S—H2SA | 109.6 |
C3—C2—H2A | 120.9 | N1S—C2S—H2SB | 109.6 |
C1—C2—H2A | 120.9 | C1Si—C2S—H2SB | 109.6 |
C2—C3—C4 | 119.5 (2) | H2SA—C2S—H2SB | 108.1 |
C2—C3—H3A | 120.2 | C4S—N2S—C3S | 111.96 (17) |
C4—C3—H3A | 120.2 | C4S—N2S—H2NA | 109.1 |
C5—C4—C3 | 118.7 (2) | C3S—N2S—H2NA | 109.8 |
C5—C4—H4A | 120.7 | C4S—N2S—H2NB | 106.1 |
C3—C4—H4A | 120.7 | C3S—N2S—H2NB | 113.8 |
N1—C5—C4 | 121.7 (2) | H2NA—N2S—H2NB | 105.9 |
N1—C5—C7 | 116.31 (19) | N2S—C3S—C4Sii | 109.72 (18) |
C4—C5—C7 | 121.97 (19) | N2S—C3S—H3SA | 109.7 |
O2—C6—O1 | 124.5 (2) | C4Sii—C3S—H3SA | 109.7 |
O2—C6—C1 | 118.08 (19) | N2S—C3S—H3SB | 109.7 |
O1—C6—C1 | 117.41 (19) | C4Sii—C3S—H3SB | 109.7 |
O3—C7—O4 | 125.9 (2) | H3SA—C3S—H3SB | 108.2 |
O3—C7—C5 | 117.38 (19) | N2S—C4S—C3Sii | 110.16 (19) |
O4—C7—C5 | 116.75 (19) | N2S—C4S—H4SA | 109.6 |
N2—C8—C9 | 122.3 (2) | C3Sii—C4S—H4SA | 109.6 |
N2—C8—C13 | 115.66 (19) | N2S—C4S—H4SB | 109.6 |
C9—C8—C13 | 122.03 (19) | C3Sii—C4S—H4SB | 109.6 |
C10—C9—C8 | 118.7 (2) | H4SA—C4S—H4SB | 108.1 |
C10—C9—H9A | 120.6 | H1WA—O1W—H1WB | 112.6 |
C8—C9—H9A | 120.6 | H2WA—O2W—H2WB | 104.8 |
C9—C10—C11 | 119.1 (2) | | |
| | | |
O5—Pb1—O1—C6 | 79.00 (18) | C1—N1—C5—C4 | −0.7 (3) |
N2—Pb1—O1—C6 | 143.04 (19) | Pb1—N1—C5—C4 | 179.99 (16) |
N1—Pb1—O1—C6 | 5.84 (17) | C1—N1—C5—C7 | 178.98 (18) |
O7—Pb1—O1—C6 | −151.39 (19) | Pb1—N1—C5—C7 | −0.4 (3) |
O3—Pb1—O1—C6 | 5.2 (2) | C3—C4—C5—N1 | −0.8 (3) |
O1—Pb1—O3—C7 | 12.71 (18) | C3—C4—C5—C7 | 179.6 (2) |
O5—Pb1—O3—C7 | −69.64 (16) | Pb1—O1—C6—O2 | 173.84 (17) |
N2—Pb1—O3—C7 | −94.99 (16) | Pb1—O1—C6—C1 | −6.9 (3) |
N1—Pb1—O3—C7 | 11.99 (15) | N1—C1—C6—O2 | −178.2 (2) |
O7—Pb1—O3—C7 | 140.15 (15) | C2—C1—C6—O2 | 3.0 (3) |
O1—Pb1—O5—C13 | 72.56 (17) | N1—C1—C6—O1 | 2.5 (3) |
N2—Pb1—O5—C13 | 1.13 (16) | C2—C1—C6—O1 | −176.3 (2) |
N1—Pb1—O5—C13 | 136.38 (17) | Pb1—O3—C7—O4 | 162.50 (18) |
O7—Pb1—O5—C13 | 1.90 (19) | Pb1—O3—C7—C5 | −16.9 (2) |
O3—Pb1—O5—C13 | −160.34 (17) | N1—C5—C7—O3 | 12.0 (3) |
O1—Pb1—O7—C14 | −76.08 (17) | C4—C5—C7—O3 | −168.4 (2) |
O5—Pb1—O7—C14 | 3.6 (2) | N1—C5—C7—O4 | −167.52 (19) |
N2—Pb1—O7—C14 | 4.43 (16) | C4—C5—C7—O4 | 12.1 (3) |
N1—Pb1—O7—C14 | −104.91 (17) | C12—N2—C8—C9 | 0.3 (3) |
O3—Pb1—O7—C14 | 145.70 (15) | Pb1—N2—C8—C9 | 176.50 (16) |
O1—Pb1—N1—C1 | −3.89 (14) | C12—N2—C8—C13 | −179.29 (18) |
O5—Pb1—N1—C1 | −103.47 (15) | Pb1—N2—C8—C13 | −3.1 (2) |
N2—Pb1—N1—C1 | −54.26 (17) | N2—C8—C9—C10 | 0.6 (3) |
O7—Pb1—N1—C1 | 26.64 (18) | C13—C8—C9—C10 | −179.9 (2) |
O3—Pb1—N1—C1 | 175.48 (17) | C8—C9—C10—C11 | −0.8 (3) |
O1—Pb1—N1—C5 | 175.48 (18) | C9—C10—C11—C12 | 0.2 (3) |
O5—Pb1—N1—C5 | 75.90 (16) | C8—N2—C12—C11 | −0.9 (3) |
N2—Pb1—N1—C5 | 125.11 (16) | Pb1—N2—C12—C11 | −176.97 (15) |
O7—Pb1—N1—C5 | −153.99 (15) | C8—N2—C12—C14 | 176.10 (18) |
O3—Pb1—N1—C5 | −5.15 (15) | Pb1—N2—C12—C14 | 0.1 (2) |
O1—Pb1—N2—C8 | −99.01 (15) | C10—C11—C12—N2 | 0.7 (3) |
O5—Pb1—N2—C8 | 1.24 (14) | C10—C11—C12—C14 | −176.2 (2) |
N1—Pb1—N2—C8 | −52.31 (16) | Pb1—O5—C13—O6 | 176.69 (16) |
O7—Pb1—N2—C8 | −178.08 (17) | Pb1—O5—C13—C8 | −3.1 (3) |
O3—Pb1—N2—C8 | 28.25 (18) | N2—C8—C13—O6 | −175.75 (19) |
O1—Pb1—N2—C12 | 77.09 (16) | C9—C8—C13—O6 | 4.7 (3) |
O5—Pb1—N2—C12 | 177.33 (17) | N2—C8—C13—O5 | 4.1 (3) |
N1—Pb1—N2—C12 | 123.78 (16) | C9—C8—C13—O5 | −175.5 (2) |
O7—Pb1—N2—C12 | −1.99 (15) | Pb1—O7—C14—O8 | 171.24 (17) |
O3—Pb1—N2—C12 | −155.65 (14) | Pb1—O7—C14—C12 | −6.1 (3) |
C5—N1—C1—C2 | 1.8 (3) | N2—C12—C14—O7 | 4.1 (3) |
Pb1—N1—C1—C2 | −178.81 (16) | C11—C12—C14—O7 | −178.8 (2) |
C5—N1—C1—C6 | −177.05 (18) | N2—C12—C14—O8 | −173.49 (19) |
Pb1—N1—C1—C6 | 2.4 (2) | C11—C12—C14—O8 | 3.5 (3) |
N1—C1—C2—C3 | −1.4 (3) | C2S—N1S—C1S—C2Si | 56.7 (3) |
C6—C1—C2—C3 | 177.3 (2) | C1S—N1S—C2S—C1Si | −56.4 (3) |
C1—C2—C3—C4 | −0.1 (3) | C4S—N2S—C3S—C4Sii | 57.4 (3) |
C2—C3—C4—C5 | 1.1 (3) | C3S—N2S—C4S—C3Sii | −57.6 (3) |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1, −y+2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1S—H1NA···O2iii | 0.89 | 1.86 | 2.744 (3) | 175 |
N1S—H1NB···O8iv | 0.91 | 1.87 | 2.774 (3) | 176 |
N2S—H2NA···O6iii | 0.86 | 1.89 | 2.748 (3) | 171 |
N2S—H2NB···O1W | 0.84 | 1.89 | 2.708 (3) | 167 |
O1W—H1WA···O4ii | 0.83 | 1.89 | 2.704 (3) | 168 |
O1W—H1WB···O3iii | 0.72 | 2.05 | 2.752 (3) | 164 |
O2W—H2WA···O8 | 0.84 | 2.03 | 2.809 (3) | 154 |
O2W—H2WB···O4v | 0.82 | 2.02 | 2.813 (3) | 161 |
Symmetry codes: (ii) −x+1, −y+2, −z; (iii) x+1, y, z; (iv) −x+1, −y+1, −z+1; (v) x+1, y, z+1. |
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