Download citation
Download citation
link to html
The title compound, {(C18H34N2O8)[Hg4I10]}n, contains two subunits, namely doubly protonated N,N,N′,N′-tetra­kis[3-(methoxy­carbon­yl)prop­yl]ethyl­enediammonium cations and macroanionic penta­iodo­dimercurate [Hg2I5]n chains. The complete cation is generated by twofold symmetry and the polymeric anion contains corner- and edge-shared HgI3 and HgI4 polyhedra.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806035380/hb2122sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806035380/hb2122Isup2.hkl
Contains datablock I

CCDC reference: 624541

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.018 Å
  • Disorder in main residue
  • R factor = 0.054
  • wR factor = 0.115
  • Data-to-parameter ratio = 20.3

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.90 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.85 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for Hg1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for Hg2A PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for Hg1A PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for Hg2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for I1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for I2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for I4 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.26 PLAT301_ALERT_3_C Main Residue Disorder ......................... 14.00 Perc. PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 18 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.11 Ratio
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 9 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

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL/NT (Bruker, 2000); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/NT; software used to prepare material for publication: SHELXL97.

Poly[N,N,N',N'-Tetrakis[3-(methoxycarbonyl)propyl]ethylenediammonium [tetra-µ-iodo-hexaiodotetramercurate]] top
Crystal data top
(C18H34N2O8)[Hg4I10]F(000) = 4280
Mr = 2477.84Dx = 3.608 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 250 reflections
a = 18.580 (5) Åθ = 2.0–25.5°
b = 16.805 (4) ŵ = 20.23 mm1
c = 14.864 (4) ÅT = 298 K
β = 100.632 (5)°Block, yellow
V = 4561 (2) Å30.11 × 0.10 × 0.06 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
4237 independent reflections
Radiation source: fine-focus sealed tube2702 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.062
ω scansθmax = 25.5°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 2220
Tmin = 0.122, Tmax = 0.290k = 2017
11521 measured reflectionsl = 1810
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)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.115H-atom parameters constrained
S = 0.98 w = 1/[σ2(Fo2) + (0.0369P)2]
where P = (Fo2 + 2Fc2)/3
4237 reflections(Δ/σ)max = 0.001
209 parametersΔρmax = 1.66 e Å3
6 restraintsΔρmin = 1.32 e Å3
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
xyzUiso*/UeqOcc. (<1)
C10.0418 (6)0.3147 (6)0.2542 (8)0.030 (3)
H1A0.05840.36840.24500.036*
H1B0.06430.29800.31540.036*
C20.0500 (8)0.2954 (7)0.0891 (8)0.041 (3)
H2A0.08830.33310.08290.050*
H2B0.00410.32420.08130.050*
C30.0453 (8)0.2320 (8)0.0141 (9)0.051 (4)
H3A0.03720.25760.04540.061*
H3B0.09130.20320.02150.061*
C40.0151 (9)0.1755 (8)0.0185 (9)0.043 (4)
C50.1482 (7)0.2389 (7)0.2110 (9)0.038 (3)
H5A0.16510.21800.15770.045*
H5B0.17540.28740.22940.045*
C60.1641 (8)0.1806 (7)0.2858 (8)0.035 (3)
H6A0.15460.20520.34150.042*
H6B0.21580.16750.29550.042*
C70.1202 (8)0.1043 (8)0.2695 (10)0.043 (4)
C80.0851 (11)0.0690 (10)0.0517 (12)0.084 (6)
H8A0.08410.03140.10000.127*
H8B0.13010.09850.06400.127*
H8C0.08180.04120.00540.127*
C90.1002 (9)0.0227 (8)0.3216 (10)0.061 (5)
H9A0.11980.05740.37140.092*
H9B0.10460.04750.26470.092*
H9C0.04960.01230.32250.092*
N10.0661 (5)0.2593 (5)0.1844 (6)0.028 (2)
H100.04020.21320.18330.033*
Hg10.3049 (5)0.0049 (5)0.5056 (10)0.090 (2)0.65 (3)
Hg20.4016 (8)0.1094 (6)0.2486 (10)0.093 (3)0.35 (3)
Hg1A0.2981 (7)0.0066 (8)0.4755 (17)0.080 (3)0.35 (3)
Hg2A0.3863 (5)0.1011 (3)0.2299 (6)0.0817 (15)0.65 (3)
I10.25297 (6)0.13689 (6)0.50906 (7)0.0627 (3)
I20.31927 (7)0.15598 (6)0.50683 (7)0.0689 (4)
I40.30375 (6)0.01951 (5)0.26976 (7)0.0566 (3)
I30.47111 (6)0.04490 (6)0.60649 (6)0.0479 (3)
I50.37510 (8)0.25573 (6)0.25774 (9)0.0741 (4)
O10.0239 (7)0.1233 (6)0.0461 (7)0.070 (3)
O20.0559 (6)0.1789 (5)0.0742 (7)0.056 (3)
O30.1397 (5)0.0500 (5)0.3308 (6)0.045 (2)
O40.0735 (7)0.0951 (6)0.2010 (8)0.078 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.028 (8)0.028 (6)0.032 (7)0.011 (5)0.005 (6)0.006 (5)
C20.046 (10)0.047 (8)0.033 (8)0.007 (7)0.014 (7)0.008 (6)
C30.037 (10)0.078 (10)0.040 (9)0.010 (8)0.015 (7)0.028 (8)
C40.056 (11)0.047 (8)0.026 (8)0.015 (7)0.004 (7)0.003 (6)
C50.016 (8)0.047 (8)0.050 (9)0.002 (6)0.005 (6)0.007 (6)
C60.041 (9)0.036 (7)0.028 (7)0.002 (6)0.006 (6)0.000 (6)
C70.031 (9)0.043 (8)0.055 (10)0.011 (7)0.007 (7)0.006 (7)
C80.092 (10)0.078 (8)0.081 (9)0.016 (8)0.011 (8)0.008 (7)
C90.064 (12)0.040 (8)0.079 (12)0.003 (8)0.007 (9)0.025 (8)
N10.020 (6)0.031 (5)0.033 (6)0.005 (4)0.008 (5)0.000 (4)
Hg10.081 (2)0.0364 (10)0.151 (5)0.0108 (13)0.015 (3)0.002 (2)
Hg20.114 (4)0.041 (2)0.115 (4)0.021 (3)0.000 (5)0.016 (2)
Hg1A0.051 (3)0.036 (2)0.150 (9)0.0001 (17)0.008 (4)0.016 (4)
Hg2A0.116 (3)0.0442 (10)0.100 (2)0.0093 (16)0.060 (3)0.0169 (13)
I10.0610 (8)0.0528 (6)0.0707 (8)0.0172 (5)0.0024 (6)0.0145 (5)
I20.0921 (10)0.0360 (5)0.0640 (7)0.0001 (6)0.0235 (6)0.0057 (5)
I40.0555 (8)0.0432 (5)0.0786 (8)0.0030 (5)0.0322 (6)0.0020 (5)
I30.0445 (7)0.0608 (6)0.0398 (5)0.0005 (5)0.0118 (4)0.0052 (4)
I50.0946 (11)0.0395 (6)0.0867 (9)0.0007 (6)0.0123 (7)0.0045 (5)
O10.087 (10)0.083 (8)0.041 (6)0.014 (7)0.018 (6)0.014 (6)
O20.057 (8)0.054 (6)0.055 (7)0.012 (5)0.008 (6)0.022 (5)
O30.042 (7)0.037 (5)0.053 (6)0.014 (5)0.003 (5)0.007 (5)
O40.101 (11)0.047 (6)0.068 (8)0.002 (6)0.031 (7)0.013 (5)
Geometric parameters (Å, º) top
C1—N11.523 (13)C8—H8B0.9600
C1—C1i1.54 (2)C8—H8C0.9600
C1—H1A0.9700C9—O31.418 (16)
C1—H1B0.9700C9—H9A0.9600
C2—N11.519 (14)C9—H9B0.9600
C2—C31.533 (18)C9—H9C0.9600
C2—H2A0.9700N1—H100.9100
C2—H2B0.9700Hg1—I22.553 (8)
C3—C41.482 (19)Hg1—I12.574 (8)
C3—H3A0.9700Hg1—I33.283 (10)
C3—H3B0.9700Hg1A—I22.570 (14)
C4—O21.222 (15)Hg1A—I12.631 (17)
C4—O11.287 (15)Hg1A—I43.11 (2)
C5—C61.471 (16)Hg2—I52.516 (9)
C5—N11.542 (16)Hg2—I3ii2.883 (9)
C5—H5A0.9700Hg2—I42.883 (13)
C5—H5B0.9700Hg2—I3iii3.086 (14)
C6—C71.515 (17)Hg2A—I52.645 (6)
C6—H6A0.9700Hg2A—I42.673 (6)
C6—H6B0.9700Hg2A—I3ii2.794 (4)
C7—O41.220 (17)Hg2A—I3iii3.383 (5)
C7—O31.294 (15)I3—Hg2Aiv2.794 (4)
C8—O11.45 (2)I3—Hg2iv2.883 (9)
C8—H8A0.9600I3—Hg2iii3.086 (14)
N1—C1—C1i111.5 (10)H8B—C8—H8C109.5
N1—C1—H1A109.3O3—C9—H9A109.5
C1i—C1—H1A109.3O3—C9—H9B109.5
N1—C1—H1B109.3H9A—C9—H9B109.5
C1i—C1—H1B109.3O3—C9—H9C109.5
H1A—C1—H1B108.0H9A—C9—H9C109.5
N1—C2—C3112.0 (10)H9B—C9—H9C109.5
N1—C2—H2A109.2C2—N1—C1111.0 (9)
C3—C2—H2A109.2C2—N1—C5110.0 (9)
N1—C2—H2B109.2C1—N1—C5111.3 (9)
C3—C2—H2B109.2C2—N1—H10108.1
H2A—C2—H2B107.9C1—N1—H10108.1
C4—C3—C2110.8 (11)C5—N1—H10108.1
C4—C3—H3A109.5I2—Hg1—I1163.6 (3)
C2—C3—H3A109.5I2—Hg1—I399.3 (3)
C4—C3—H3B109.5I1—Hg1—I394.6 (3)
C2—C3—H3B109.5I2—Hg1a—I1154.8 (10)
H3A—C3—H3B108.1I2—Hg1a—I4106.5 (8)
O2—C4—O1121.9 (14)I1—Hg1a—I497.3 (5)
O2—C4—C3124.7 (12)I5—Hg2—I3ii121.7 (3)
O1—C4—C3113.4 (12)I5—Hg2—I4126.5 (4)
C6—C5—N1113.1 (10)I3ii—Hg2—I4100.0 (4)
C6—C5—H5A109.0I5—Hg2—I3iii116.0 (7)
N1—C5—H5A109.0I3ii—Hg2—I3iii89.4 (3)
C6—C5—H5B109.0I4—Hg2—I3iii94.4 (2)
N1—C5—H5B109.0I5—Hg2a—I4130.18 (15)
H5A—C5—H5B107.8I5—Hg2a—I3ii120.32 (14)
C5—C6—C7114.6 (12)I4—Hg2a—I3ii107.8 (2)
C5—C6—H6A108.6I5—Hg2a—I3iii103.6 (2)
C7—C6—H6A108.6I3ii—Hg2a—I3iii85.2 (2)
C5—C6—H6B108.6I4—Hg2a—I3iii92.0 (2)
C7—C6—H6B108.6Hg2a—I4—Hg1a103.6 (4)
H6A—C6—H6B107.6Hg2—I4—Hg1a97.9 (4)
O4—C7—O3124.2 (13)Hg2aiv—I3—Hg2iii82.8 (3)
O4—C7—C6121.3 (13)Hg2iv—I3—Hg2iii75.3 (5)
O3—C7—C6114.3 (13)Hg2aiv—I3—Hg177.8 (4)
O1—C8—H8A109.5Hg2iv—I3—Hg185.4 (5)
O1—C8—H8B109.5Hg2iii—I3—Hg1160.6 (2)
H8A—C8—H8B109.5C4—O1—C8117.5 (12)
O1—C8—H8C109.5C7—O3—C9117.8 (12)
H8A—C8—H8C109.5
Symmetry codes: (i) x, y, z+1/2; (ii) x, y, z1/2; (iii) x+1, y, z+1; (iv) x, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H10···O20.912.252.876 (14)125
N1—H10···O40.912.082.771 (13)132
C6—H6A···O2i0.972.443.150 (15)129
Symmetry code: (i) x, y, z+1/2.
 

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