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The title compound, [Ag4(C8H4O4)2{H2N(CH2)6}3]·2H2O, is an AgI tetranuclear complex. Four AgI atoms, three hexa­methyl­enedi­amine mol­ecules, and two terephthalate dianions constitute a chain-like tetranuclear silver(I) complex. The complex lies on a center of symmetry, located at the mid-point of the central C—C bond. The two different kinds of AgI atoms are both in a linear environment. One kind of Ag atom is coordinated by two N atoms from different amine ligands, and the other is coordinated by an O atom from a carboxyl­ate group and by a N atom from an amine ligand. Adjacent complexes are joined together by weak Ag...Ag interactions to form ladder-like ribbons, which are further linked by hydrogen bonds to form a three-dimensional structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803020373/om6175sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803020373/om6175Isup2.hkl
Contains datablock I

CCDC reference: 225686

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.037
  • wR factor = 0.093
  • Data-to-parameter ratio = 15.6

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.97
Alert level B PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... C14
Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT213_ALERT_2_C Atom N2 has ADP max/min Ratio ............. 3.50 prolat PLAT220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 3.01 Ratio PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor .... 2.31 PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2A ... ? PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 9 N3 -AG1 -N1 -C9 -49.00 3.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 11 N1 -AG1 -N3 -C15 -131.00 3.00 1.555 1.555 1.555 1.555 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
1 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 11 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 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 5 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1997); software used to prepare material for publication: SHELXTL.

Tris(1,6-diaminohexane)diterephthalatotetrasilver(I) dihydrate top
Crystal data top
[Ag4(C8H4O4)2(C6H14N2)3]·2H2OZ = 2
Mr = 572.18F(000) = 574
Triclinic, P1Dx = 1.893 Mg m3
a = 7.220 (1) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.928 (2) ÅCell parameters from 4208 reflections
c = 13.919 (3) Åθ = 2.8–25.9°
α = 110.08 (3)°µ = 1.98 mm1
β = 98.73 (3)°T = 293 K
γ = 96.31 (3)°Rod, colorless
V = 1003.9 (3) Å30.38 × 0.38 × 0.30 mm
Data collection top
Siemens SMART CCD area-detector
diffractometer
3814 independent reflections
Radiation source: fine-focus sealed tube3353 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.015
φ and ω scansθmax = 26.0°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 86
Tmin = 0.490, Tmax = 0.552k = 1213
4537 measured reflectionsl = 1717
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.093 w = 1/[σ2(Fo2) + (0.0429P)2 + 1.1362P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.001
3814 reflectionsΔρmax = 0.93 e Å3
245 parametersΔρmin = 0.95 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0038 (6)
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*/Ueq
Ag10.45582 (5)0.47516 (3)0.32966 (2)0.04479 (13)
Ag20.13054 (6)0.37910 (4)0.13754 (3)0.06196 (16)
O30.0277 (5)0.1945 (3)0.1412 (3)0.0552 (8)
O20.0853 (5)0.3665 (3)0.3071 (3)0.0609 (9)
C100.5037 (6)0.1375 (4)0.2084 (3)0.0357 (8)
H10A0.40430.16490.24530.080*
H10B0.61180.13810.25820.080*
C50.0281 (5)0.0475 (4)0.2278 (3)0.0362 (8)
C40.0158 (6)0.0247 (4)0.3207 (3)0.0398 (9)
H4A0.01820.09840.38610.080*
C130.3548 (6)0.2465 (4)0.0998 (3)0.0418 (9)
H13A0.45560.26730.06240.080*
H13B0.24200.25390.05030.080*
N10.6357 (5)0.3690 (3)0.2367 (3)0.0425 (8)
H1A0.73610.36220.28040.080*
H1B0.68070.41890.20280.080*
N30.2685 (5)0.5793 (3)0.4171 (3)0.0450 (8)
H3B0.22050.52980.45040.080*
H3C0.17080.58590.37160.080*
C60.0808 (6)0.0600 (4)0.1339 (3)0.0393 (9)
H6A0.08970.04570.06920.080*
C70.1220 (6)0.1863 (4)0.1337 (3)0.0396 (9)
H7A0.16160.25940.06820.080*
C30.0523 (6)0.1025 (4)0.3196 (3)0.0389 (9)
H3A0.04050.11670.38440.080*
C120.4085 (6)0.1061 (4)0.1781 (3)0.0376 (9)
H12A0.52420.09850.22560.080*
H12B0.31040.08770.21770.080*
C160.4073 (6)0.8096 (4)0.4454 (3)0.0440 (10)
H16A0.50970.78190.41130.080*
H16B0.30270.80850.39330.080*
O10.2176 (6)0.4402 (3)0.1402 (2)0.0682 (10)
C170.4709 (7)0.9501 (4)0.5241 (3)0.0482 (10)
H17A0.57760.95120.57490.080*
H17B0.36970.97620.55980.080*
C20.1057 (5)0.2098 (4)0.2257 (3)0.0348 (8)
C90.5581 (6)0.2347 (4)0.1580 (3)0.0399 (9)
H9A0.44790.23860.11160.080*
H9B0.65140.20420.11730.080*
C80.0173 (6)0.1861 (4)0.2290 (4)0.0425 (9)
C150.3453 (7)0.7136 (4)0.4955 (3)0.0471 (10)
H15A0.45300.70880.54310.080*
H15B0.25100.74570.53490.080*
O40.0377 (6)0.2814 (3)0.3106 (3)0.0660 (10)
C110.4361 (6)0.0031 (4)0.1285 (3)0.0382 (9)
H11A0.52760.02510.08480.080*
H11B0.31780.00610.08490.080*
C140.3193 (7)0.3442 (4)0.1527 (3)0.0471 (10)
H14A0.21410.32480.18670.080*
H14B0.42940.33030.20590.080*
C10.1397 (6)0.3493 (4)0.2246 (3)0.0416 (9)
N20.2714 (12)0.4793 (4)0.0868 (4)0.127 (3)
H2A0.38340.50440.07580.080*
H2B0.20410.48620.02460.080*
O1W0.2084 (5)0.3810 (4)0.4810 (3)0.0776 (11)
H1WA0.16930.37640.41720.080*
H1WB0.16620.32730.54760.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.0578 (2)0.03001 (19)0.0447 (2)0.00802 (14)0.01112 (15)0.01095 (14)
Ag20.0913 (3)0.0387 (2)0.0553 (2)0.00989 (18)0.0051 (2)0.02711 (18)
O30.071 (2)0.0385 (17)0.060 (2)0.0016 (15)0.0111 (16)0.0273 (15)
O20.082 (2)0.0466 (19)0.058 (2)0.0028 (16)0.0015 (17)0.0349 (16)
C100.041 (2)0.0270 (19)0.038 (2)0.0019 (15)0.0110 (16)0.0105 (16)
C50.0336 (19)0.031 (2)0.046 (2)0.0040 (15)0.0081 (16)0.0171 (17)
C40.046 (2)0.033 (2)0.040 (2)0.0087 (17)0.0093 (17)0.0121 (17)
C130.058 (3)0.029 (2)0.040 (2)0.0010 (18)0.0128 (19)0.0162 (17)
N10.049 (2)0.0255 (17)0.051 (2)0.0006 (14)0.0140 (16)0.0113 (15)
N30.052 (2)0.0355 (19)0.046 (2)0.0046 (15)0.0109 (16)0.0124 (16)
C60.045 (2)0.036 (2)0.040 (2)0.0041 (17)0.0075 (17)0.0193 (18)
C70.047 (2)0.032 (2)0.039 (2)0.0026 (17)0.0053 (17)0.0150 (17)
C30.048 (2)0.038 (2)0.036 (2)0.0095 (17)0.0114 (17)0.0183 (17)
C120.046 (2)0.030 (2)0.037 (2)0.0056 (16)0.0095 (17)0.0125 (16)
C160.058 (3)0.032 (2)0.039 (2)0.0072 (18)0.0113 (19)0.0090 (17)
O10.119 (3)0.0326 (17)0.0449 (18)0.0114 (18)0.0104 (19)0.0144 (15)
C170.062 (3)0.034 (2)0.042 (2)0.0029 (19)0.011 (2)0.0083 (19)
C20.036 (2)0.030 (2)0.041 (2)0.0044 (15)0.0088 (16)0.0159 (17)
C90.051 (2)0.027 (2)0.041 (2)0.0023 (17)0.0129 (18)0.0121 (17)
C80.039 (2)0.035 (2)0.056 (3)0.0073 (17)0.0064 (18)0.022 (2)
C150.063 (3)0.034 (2)0.039 (2)0.0050 (19)0.014 (2)0.0071 (18)
O40.103 (3)0.0320 (17)0.057 (2)0.0030 (17)0.0073 (19)0.0154 (16)
C110.049 (2)0.027 (2)0.038 (2)0.0033 (16)0.0090 (17)0.0113 (16)
C140.065 (3)0.031 (2)0.051 (3)0.0056 (19)0.020 (2)0.0185 (19)
C10.048 (2)0.033 (2)0.046 (2)0.0029 (17)0.0124 (19)0.0170 (19)
N20.288 (9)0.034 (3)0.050 (3)0.028 (4)0.052 (4)0.012 (2)
O1W0.081 (3)0.091 (3)0.050 (2)0.019 (2)0.0043 (18)0.026 (2)
Geometric parameters (Å, º) top
Ag1—N32.120 (4)C3—C21.388 (5)
Ag1—N12.125 (3)C3—H3A0.9600
Ag1—Ag23.0646 (14)C12—C111.518 (5)
Ag2—O32.092 (3)C12—H12A0.9600
Ag2—N2i2.133 (4)C12—H12B0.9600
O3—C81.269 (5)C16—C151.510 (6)
O2—C11.240 (5)C16—C171.518 (6)
C10—C91.510 (5)C16—H16A0.9600
C10—C111.527 (5)C16—H16B0.9600
C10—H10A0.9600O1—C11.247 (5)
C10—H10B0.9600C17—C17ii1.517 (8)
C5—C61.389 (5)C17—H17A0.9600
C5—C41.390 (6)C17—H17B0.9600
C5—C81.508 (5)C2—C11.511 (5)
C4—C31.381 (6)C9—H9A0.9600
C4—H4A0.9600C9—H9B0.9600
C13—C121.512 (5)C8—O41.225 (5)
C13—C141.512 (5)C15—H15A0.9601
C13—H13A0.9600C15—H15B0.9600
C13—H13B0.9600C11—H11A0.9600
N1—C91.483 (5)C11—H11B0.9600
N1—H1A0.8999C14—N21.415 (6)
N1—H1B0.9000C14—H14A0.9600
N3—C151.480 (5)C14—H14B0.9600
N3—H3B0.9001N2—Ag2iii2.133 (4)
N3—H3C0.9000N2—H2A0.9000
C6—C71.378 (5)N2—H2B0.9000
C6—H6A0.9600O1W—H1WA0.9876
C7—C21.382 (5)O1W—H1WB0.8931
C7—H7A0.9600
N3—Ag1—N1177.80 (13)C15—C16—C17112.4 (3)
N3—Ag1—Ag287.93 (10)C15—C16—H16A109.4
N1—Ag1—Ag289.89 (10)C17—C16—H16A109.3
O3—Ag2—N2i158.96 (18)C15—C16—H16B108.9
O3—Ag2—Ag198.98 (10)C17—C16—H16B108.8
N2i—Ag2—Ag187.55 (18)H16A—C16—H16B108.0
C8—O3—Ag2118.5 (3)C17ii—C17—C16113.8 (4)
C9—C10—C11112.2 (3)C17ii—C17—H17A108.4
C9—C10—H10A109.2C16—C17—H17A108.4
C11—C10—H10A109.3C17ii—C17—H17B109.3
C9—C10—H10B109.1C16—C17—H17B108.9
C11—C10—H10B109.0H17A—C17—H17B107.8
H10A—C10—H10B108.0C7—C2—C3118.5 (3)
C6—C5—C4118.7 (4)C7—C2—C1120.9 (4)
C6—C5—C8120.7 (4)C3—C2—C1120.6 (3)
C4—C5—C8120.6 (4)N1—C9—C10111.8 (3)
C3—C4—C5120.6 (4)N1—C9—H9A109.2
C3—C4—H4A119.9C10—C9—H9A109.1
C5—C4—H4A119.5N1—C9—H9B109.5
C12—C13—C14111.5 (3)C10—C9—H9B109.2
C12—C13—H13A109.2H9A—C9—H9B108.0
C14—C13—H13A109.4O4—C8—O3124.3 (4)
C12—C13—H13B109.4O4—C8—C5120.2 (4)
C14—C13—H13B109.2O3—C8—C5115.5 (4)
H13A—C13—H13B108.1N3—C15—C16111.9 (3)
C9—N1—Ag1119.4 (3)N3—C15—H15A108.7
C9—N1—H1A107.4C16—C15—H15A108.9
Ag1—N1—H1A107.5N3—C15—H15B109.9
C9—N1—H1B107.4C16—C15—H15B109.3
Ag1—N1—H1B107.5H15A—C15—H15B108.0
H1A—N1—H1B107.0C12—C11—C10113.3 (3)
C15—N3—Ag1118.1 (3)C12—C11—H11A108.8
C15—N3—H3B107.6C10—C11—H11A109.0
Ag1—N3—H3B107.8C12—C11—H11B108.9
C15—N3—H3C107.8C10—C11—H11B108.9
Ag1—N3—H3C107.8H11A—C11—H11B107.9
H3B—N3—H3C107.2N2—C14—C13116.3 (4)
C7—C6—C5120.2 (4)N2—C14—H14A106.0
C7—C6—H6A120.2C13—C14—H14A108.3
C5—C6—H6A119.6N2—C14—H14B110.3
C6—C7—C2121.3 (4)C13—C14—H14B108.0
C6—C7—H7A119.3H14A—C14—H14B107.5
C2—C7—H7A119.4O2—C1—O1124.2 (4)
C4—C3—C2120.6 (4)O2—C1—C2117.8 (4)
C4—C3—H3A119.6O1—C1—C2118.0 (4)
C2—C3—H3A119.8C14—N2—Ag2iii120.5 (3)
C13—C12—C11113.6 (3)C14—N2—H2A104.9
C13—C12—H12A108.9Ag2iii—N2—H2A105.9
C11—C12—H12A108.8C14—N2—H2B109.0
C13—C12—H12B108.7Ag2iii—N2—H2B108.7
C11—C12—H12B108.8H2A—N2—H2B107.2
H12A—C12—H12B107.8H1WA—O1W—H1WB129.7
N3—Ag1—Ag2—O396.44 (14)C4—C3—C2—C70.2 (6)
N1—Ag1—Ag2—O383.88 (13)C4—C3—C2—C1178.1 (4)
N3—Ag1—Ag2—N2i103.7 (2)Ag1—N1—C9—C1065.5 (4)
N1—Ag1—Ag2—N2i76.0 (2)C11—C10—C9—N1176.2 (3)
N2i—Ag2—O3—C8147.7 (6)Ag2—O3—C8—O410.9 (6)
Ag1—Ag2—O3—C840.8 (3)Ag2—O3—C8—C5170.7 (2)
C6—C5—C4—C31.1 (6)C6—C5—C8—O4169.8 (4)
C8—C5—C4—C3178.2 (4)C4—C5—C8—O411.0 (6)
N3—Ag1—N1—C949 (3)C6—C5—C8—O38.7 (6)
Ag2—Ag1—N1—C941.2 (3)C4—C5—C8—O3170.6 (4)
N1—Ag1—N3—C15131 (3)Ag1—N3—C15—C1664.9 (4)
Ag2—Ag1—N3—C15139.6 (3)C17—C16—C15—N3175.2 (4)
C4—C5—C6—C70.7 (6)C13—C12—C11—C10176.0 (3)
C8—C5—C6—C7180.0 (4)C9—C10—C11—C12171.4 (3)
C5—C6—C7—C22.3 (6)C12—C13—C14—N2178.8 (5)
C5—C4—C3—C21.3 (6)C7—C2—C1—O2165.2 (4)
C14—C13—C12—C11177.1 (4)C3—C2—C1—O213.0 (6)
C15—C16—C17—C17ii178.4 (5)C7—C2—C1—O113.6 (6)
C6—C7—C2—C32.0 (6)C3—C2—C1—O1168.2 (4)
C6—C7—C2—C1176.3 (4)C13—C14—N2—Ag2iii159.7 (4)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y+2, z+1; (iii) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O4iv0.902.473.283 (5)151
N1—H1B···O1v0.902.133.023 (5)172
N1—H1B···O2v0.902.553.090 (5)119
N3—H3B···O1Wvi0.902.152.998 (5)157
N3—H3C···O2i0.902.132.997 (5)163
N2—H2B···O1vii0.902.182.924 (6)140
O1W—H1WA···O20.991.762.749 (5)177
O1W—H1WB···O4vi0.891.922.751 (5)155
Symmetry codes: (i) x, y+1, z; (iv) x+1, y, z; (v) x+1, y+1, z; (vi) x, y, z+1; (vii) x, y1, z.
 

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