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In the title clathrate complex, {[Sn2(CH3)6(C2N2S3)(C10H8N2)]·C10H8N2}n, two independent Sn atoms are five-coordinated in a distorted trigonal–bipyramidal geometry. The asymmetric unit contains two independent 4,4′-bipyridine systems, one of which bridges two independent Sn atoms [Sn—N = 2.588 (7) and 2.591 (7) Å], leading to the formation a one-dimensional polymeric zigzag chain.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806042899/cv2131sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806042899/cv2131Isup2.hkl
Contains datablock I

CCDC reference: 627473

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.014 Å
  • R factor = 0.036
  • wR factor = 0.092
  • Data-to-parameter ratio = 11.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.95 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for S2 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C10 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Sn1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C11 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 14
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 0.949 Tmax scaled 0.585 Tmin scaled 0.466 REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 25.01 From the CIF: _reflns_number_total 4003 Count of symmetry unique reflns 2920 Completeness (_total/calc) 137.09% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1083 Fraction of Friedel pairs measured 0.371 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

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

catena-Poly[[[trimethyltin(IV)]-µ-4,4'-bipyridyl-κ2N:N'-[trimethyltin(IV)]- µ-1,3,4-thiadiazole-2,5(3H)-dithionato(2-)-κ2N3:S5] 4,4'-bipyridine clathrate] top
Crystal data top
[Sn2(CH3)6(C2N2S3)(C10H8N2)]·C10H8N2F(000) = 784
Mr = 788.17Dx = 1.583 Mg m3
Monoclinic, PcMo Kα radiation, λ = 0.71073 Å
a = 10.886 (5) ÅCell parameters from 3491 reflections
b = 11.525 (5) Åθ = 2.4–24.7°
c = 13.236 (6) ŵ = 1.73 mm1
β = 95.249 (6)°T = 298 K
V = 1653.6 (13) Å3Block, colourless
Z = 20.48 × 0.45 × 0.31 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
4003 independent reflections
Radiation source: fine-focus sealed tube3440 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.061
φ and ω scansθmax = 25.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1112
Tmin = 0.491, Tmax = 0.617k = 1313
8311 measured reflectionsl = 1513
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)] = 0.036H-atom parameters constrained
wR(F2) = 0.092 w = 1/[σ2(Fo2) + (0.0332P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
4003 reflectionsΔρmax = 0.76 e Å3
352 parametersΔρmin = 0.68 e Å3
2 restraintsAbsolute structure: Flack (1983), 1083 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.02 (3)
Special details top

Experimental. Analysis, calculated for C84H60O10F16Sn4: C 42.66, H 4.35, N 10.66; found: C 42.43, H 4.48, N 10.49. The elemental analyses were performed with PERKIN ELMER MODEL 2400 SERIES II.

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
Sn10.38379 (5)0.47796 (4)0.97654 (4)0.04496 (17)
Sn20.85269 (5)0.39205 (5)0.75091 (4)0.04262 (16)
N10.6540 (6)0.5467 (6)0.8555 (6)0.0476 (18)
N20.7723 (6)0.5486 (5)0.8250 (5)0.0429 (16)
N30.2715 (7)0.2916 (6)1.0268 (5)0.0492 (18)
N40.0481 (7)0.2108 (6)1.1759 (6)0.0471 (17)
N50.8027 (11)0.8740 (8)0.4590 (8)0.085 (3)
N60.3368 (9)1.0333 (10)0.7765 (8)0.078 (3)
S10.7431 (2)0.74312 (17)0.90677 (18)0.0513 (5)
S20.4846 (2)0.6756 (2)0.9437 (2)0.0636 (7)
S30.9816 (2)0.6751 (2)0.8250 (2)0.0616 (6)
C10.6240 (8)0.6425 (7)0.8968 (7)0.048 (2)
C20.8359 (7)0.6446 (6)0.8477 (6)0.0370 (17)
C30.3495 (11)0.4253 (9)0.8240 (8)0.074 (3)
H3A0.27840.46540.79320.111*
H3B0.33480.34320.82130.111*
H3C0.41980.44340.78800.111*
C40.5349 (9)0.4057 (9)1.0675 (9)0.072 (3)
H4A0.53830.43841.13440.108*
H4B0.61000.42281.03790.108*
H4C0.52470.32311.07150.108*
C50.2349 (8)0.5716 (8)1.0367 (9)0.062 (3)
H5A0.25840.59231.10600.093*
H5B0.16270.52351.03330.093*
H5C0.21750.64070.99740.093*
C60.9881 (9)0.3637 (8)0.8738 (8)0.066 (3)
H6A0.95220.32150.92630.098*
H6B1.01840.43700.90000.098*
H6C1.05510.31970.85080.098*
C70.6828 (8)0.3003 (8)0.7393 (9)0.064 (3)
H7A0.67270.26200.80240.095*
H7B0.68280.24360.68610.095*
H7C0.61600.35370.72400.095*
C80.8904 (10)0.4822 (7)0.6171 (7)0.055 (2)
H8A0.81680.48580.57130.083*
H8B0.95360.44200.58500.083*
H8C0.91770.55950.63440.083*
C90.2068 (10)0.2896 (8)1.1084 (8)0.067 (3)
H90.20430.35691.14690.081*
C100.1430 (11)0.1927 (9)1.1390 (8)0.069 (3)
H100.10150.19591.19740.083*
C110.1415 (8)0.0932 (7)1.0832 (6)0.038 (2)
C120.2062 (11)0.0962 (8)0.9981 (8)0.058 (3)
H120.20900.03060.95750.070*
C130.2656 (9)0.1942 (8)0.9734 (8)0.062 (3)
H130.30550.19300.91420.075*
C140.0409 (10)0.1127 (8)1.2325 (8)0.062 (3)
H140.07680.11221.29360.074*
C150.0168 (10)0.0144 (8)1.2035 (8)0.056 (3)
H150.01870.05091.24490.067*
C160.0729 (8)0.0105 (6)1.1132 (7)0.039 (2)
C170.0601 (9)0.1107 (7)1.0548 (7)0.053 (2)
H170.09110.11250.99160.063*
C180.0031 (9)0.2057 (8)1.0885 (7)0.056 (2)
H180.00040.27171.04800.068*
C190.8020 (10)0.8317 (10)0.5515 (10)0.075 (3)
H190.86370.77940.57360.090*
C200.7148 (9)0.8603 (9)0.6185 (8)0.060 (2)
H200.72030.82930.68360.071*
C210.6177 (9)0.9373 (7)0.5855 (7)0.052 (2)
C220.6178 (12)0.9781 (9)0.4891 (10)0.080 (3)
H220.55531.02730.46260.095*
C230.7119 (15)0.9460 (10)0.4299 (10)0.094 (4)
H230.71060.97760.36520.113*
C240.3754 (12)1.1020 (10)0.7061 (11)0.082 (4)
H240.33841.17460.69860.098*
C250.4643 (9)1.0767 (8)0.6434 (8)0.061 (3)
H250.48651.13080.59620.073*
C260.5211 (9)0.9689 (7)0.6512 (7)0.050 (2)
C270.4814 (10)0.8945 (9)0.7231 (8)0.062 (3)
H270.51590.82090.73080.075*
C280.3908 (11)0.9283 (11)0.7840 (10)0.081 (3)
H280.36630.87630.83200.097*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.0436 (3)0.0497 (3)0.0423 (3)0.0034 (3)0.0082 (2)0.0007 (3)
Sn20.0403 (3)0.0481 (3)0.0403 (3)0.0016 (3)0.0079 (2)0.0025 (3)
N10.041 (4)0.049 (4)0.054 (5)0.003 (3)0.014 (4)0.001 (4)
N20.050 (4)0.040 (4)0.040 (4)0.006 (3)0.014 (3)0.005 (3)
N30.061 (5)0.050 (4)0.038 (4)0.008 (3)0.015 (3)0.006 (3)
N40.050 (4)0.039 (4)0.056 (5)0.002 (3)0.023 (4)0.003 (3)
N50.112 (9)0.073 (6)0.077 (7)0.002 (6)0.040 (7)0.002 (5)
N60.067 (6)0.106 (8)0.063 (6)0.008 (6)0.017 (5)0.023 (6)
S10.0592 (14)0.0408 (11)0.0557 (14)0.0051 (10)0.0148 (11)0.0043 (10)
S20.0562 (14)0.0460 (13)0.093 (2)0.0048 (11)0.0325 (14)0.0016 (13)
S30.0561 (14)0.0712 (15)0.0604 (16)0.0202 (12)0.0210 (12)0.0075 (13)
C10.053 (5)0.045 (5)0.046 (5)0.002 (4)0.013 (4)0.001 (4)
C20.046 (4)0.037 (4)0.028 (4)0.003 (3)0.006 (3)0.006 (3)
C30.089 (8)0.088 (7)0.049 (6)0.028 (6)0.022 (6)0.007 (5)
C40.048 (6)0.075 (6)0.090 (8)0.003 (5)0.008 (5)0.032 (6)
C50.030 (5)0.072 (6)0.087 (8)0.015 (4)0.019 (5)0.003 (6)
C60.065 (6)0.064 (5)0.064 (7)0.004 (5)0.018 (5)0.002 (5)
C70.050 (5)0.049 (5)0.093 (8)0.007 (4)0.011 (5)0.008 (5)
C80.075 (7)0.054 (5)0.038 (5)0.004 (5)0.015 (5)0.001 (4)
C90.093 (8)0.053 (6)0.060 (6)0.015 (5)0.028 (6)0.012 (5)
C100.097 (8)0.060 (6)0.058 (6)0.024 (5)0.049 (6)0.018 (5)
C110.045 (5)0.037 (4)0.032 (5)0.003 (4)0.011 (4)0.001 (4)
C120.079 (7)0.049 (5)0.052 (6)0.005 (5)0.036 (5)0.004 (4)
C130.075 (7)0.058 (6)0.061 (6)0.009 (5)0.039 (5)0.005 (5)
C140.082 (7)0.056 (5)0.052 (6)0.011 (5)0.031 (5)0.005 (5)
C150.074 (7)0.047 (5)0.050 (6)0.004 (4)0.026 (5)0.001 (4)
C160.043 (5)0.038 (4)0.039 (5)0.003 (3)0.017 (4)0.002 (4)
C170.066 (6)0.053 (5)0.042 (5)0.016 (4)0.020 (4)0.008 (4)
C180.065 (6)0.056 (5)0.050 (6)0.004 (5)0.012 (5)0.015 (5)
C190.061 (6)0.074 (7)0.091 (10)0.004 (5)0.018 (6)0.002 (7)
C200.057 (6)0.070 (6)0.052 (6)0.008 (5)0.007 (5)0.001 (5)
C210.067 (6)0.040 (4)0.048 (6)0.007 (4)0.006 (4)0.005 (4)
C220.098 (9)0.070 (7)0.070 (8)0.011 (6)0.009 (7)0.013 (6)
C230.146 (13)0.072 (8)0.070 (9)0.009 (8)0.047 (9)0.019 (7)
C240.087 (9)0.068 (7)0.090 (10)0.011 (6)0.006 (8)0.016 (7)
C250.075 (7)0.047 (5)0.060 (6)0.006 (5)0.002 (5)0.010 (5)
C260.058 (6)0.048 (5)0.043 (5)0.003 (4)0.003 (4)0.010 (4)
C270.067 (7)0.070 (6)0.049 (6)0.007 (5)0.001 (5)0.003 (5)
C280.078 (8)0.100 (9)0.065 (8)0.007 (7)0.007 (6)0.001 (7)
Geometric parameters (Å, º) top
Sn1—C32.109 (10)C7—H7B0.9600
Sn1—C42.118 (9)C7—H7C0.9600
Sn1—C52.158 (9)C8—H8A0.9600
Sn1—S22.582 (3)C8—H8B0.9600
Sn1—N32.588 (7)C8—H8C0.9600
Sn2—C62.119 (9)C9—C101.394 (14)
Sn2—C72.124 (9)C9—H90.9300
Sn2—C82.126 (9)C10—C111.364 (12)
Sn2—N22.267 (6)C10—H100.9300
Sn2—N4i2.591 (7)C11—C121.382 (13)
N1—C11.287 (11)C11—C161.482 (11)
N1—N21.384 (9)C12—C131.356 (13)
N2—C21.325 (10)C12—H120.9300
N3—C131.325 (11)C13—H130.9300
N3—C91.342 (12)C14—C151.367 (13)
N4—C181.330 (12)C14—H140.9300
N4—C141.355 (11)C15—C161.392 (14)
N4—Sn2ii2.591 (7)C15—H150.9300
N5—C191.318 (16)C16—C171.390 (11)
N5—C231.320 (16)C17—C181.354 (13)
N6—C241.320 (16)C17—H170.9300
N6—C281.345 (15)C18—H180.9300
S1—C11.736 (9)C19—C201.397 (15)
S1—C21.751 (8)C19—H190.9300
S2—C11.734 (9)C20—C211.418 (13)
S3—C21.679 (8)C20—H200.9300
C3—H3A0.9600C21—C221.360 (15)
C3—H3B0.9600C21—C261.470 (14)
C3—H3C0.9600C22—C231.395 (18)
C4—H4A0.9600C22—H220.9300
C4—H4B0.9600C23—H230.9300
C4—H4C0.9600C24—C251.363 (18)
C5—H5A0.9600C24—H240.9300
C5—H5B0.9600C25—C261.387 (13)
C5—H5C0.9600C25—H250.9300
C6—H6A0.9600C26—C271.380 (14)
C6—H6B0.9600C27—C281.385 (16)
C6—H6C0.9600C27—H270.9300
C7—H7A0.9600C28—H280.9300
C3—Sn1—C4119.4 (5)H7A—C7—H7C109.5
C3—Sn1—C5115.1 (4)H7B—C7—H7C109.5
C4—Sn1—C5123.9 (5)Sn2—C8—H8A109.5
C3—Sn1—S297.7 (3)Sn2—C8—H8B109.5
C4—Sn1—S297.0 (3)H8A—C8—H8B109.5
C5—Sn1—S288.0 (3)Sn2—C8—H8C109.5
C3—Sn1—N387.8 (3)H8A—C8—H8C109.5
C4—Sn1—N383.6 (3)H8B—C8—H8C109.5
C5—Sn1—N386.1 (3)N3—C9—C10124.0 (9)
S2—Sn1—N3173.30 (17)N3—C9—H9118.0
C6—Sn2—C7121.3 (4)C10—C9—H9118.0
C6—Sn2—C8122.8 (4)C11—C10—C9119.8 (9)
C7—Sn2—C8114.6 (4)C11—C10—H10120.1
C6—Sn2—N293.4 (3)C9—C10—H10120.1
C7—Sn2—N293.4 (3)C10—C11—C12116.0 (9)
C8—Sn2—N294.8 (3)C10—C11—C16120.9 (8)
C6—Sn2—N4i83.4 (3)C12—C11—C16123.1 (8)
C7—Sn2—N4i87.8 (3)C13—C12—C11120.5 (9)
C8—Sn2—N4i87.5 (3)C13—C12—H12119.7
N2—Sn2—N4i176.8 (3)C11—C12—H12119.7
C1—N1—N2112.9 (7)N3—C13—C12125.2 (9)
C2—N2—N1115.3 (6)N3—C13—H13117.4
C2—N2—Sn2123.3 (5)C12—C13—H13117.4
N1—N2—Sn2121.3 (5)N4—C14—C15122.8 (9)
C13—N3—C9114.3 (8)N4—C14—H14118.6
C13—N3—Sn1124.5 (6)C15—C14—H14118.6
C9—N3—Sn1121.1 (6)C14—C15—C16121.1 (9)
C18—N4—C14115.9 (8)C14—C15—H15119.5
C18—N4—Sn2ii126.3 (6)C16—C15—H15119.5
C14—N4—Sn2ii117.8 (6)C17—C16—C15114.9 (8)
C19—N5—C23115.8 (11)C17—C16—C11123.2 (8)
C24—N6—C28115.3 (11)C15—C16—C11121.8 (7)
C1—S1—C289.4 (4)C18—C17—C16120.9 (9)
C1—S2—Sn1105.4 (3)C18—C17—H17119.5
N1—C1—S2127.3 (7)C16—C17—H17119.5
N1—C1—S1112.9 (6)N4—C18—C17124.3 (9)
S2—C1—S1119.8 (5)N4—C18—H18117.8
N2—C2—S3128.1 (6)C17—C18—H18117.8
N2—C2—S1109.4 (6)N5—C19—C20124.4 (11)
S3—C2—S1122.5 (4)N5—C19—H19117.8
Sn1—C3—H3A109.5C20—C19—H19117.8
Sn1—C3—H3B109.5C19—C20—C21118.9 (10)
H3A—C3—H3B109.5C19—C20—H20120.6
Sn1—C3—H3C109.5C21—C20—H20120.6
H3A—C3—H3C109.5C22—C21—C20116.1 (10)
H3B—C3—H3C109.5C22—C21—C26122.1 (9)
Sn1—C4—H4A109.5C20—C21—C26121.8 (8)
Sn1—C4—H4B109.5C21—C22—C23119.9 (11)
H4A—C4—H4B109.5C21—C22—H22120.0
Sn1—C4—H4C109.5C23—C22—H22120.0
H4A—C4—H4C109.5N5—C23—C22124.8 (11)
H4B—C4—H4C109.5N5—C23—H23117.6
Sn1—C5—H5A109.5C22—C23—H23117.6
Sn1—C5—H5B109.5N6—C24—C25126.2 (11)
H5A—C5—H5B109.5N6—C24—H24116.9
Sn1—C5—H5C109.5C25—C24—H24116.9
H5A—C5—H5C109.5C24—C25—C26118.9 (11)
H5B—C5—H5C109.5C24—C25—H25120.6
Sn2—C6—H6A109.5C26—C25—H25120.6
Sn2—C6—H6B109.5C27—C26—C25116.2 (10)
H6A—C6—H6B109.5C27—C26—C21122.7 (8)
Sn2—C6—H6C109.5C25—C26—C21121.1 (9)
H6A—C6—H6C109.5C26—C27—C28120.8 (10)
H6B—C6—H6C109.5C26—C27—H27119.6
Sn2—C7—H7A109.5C28—C27—H27119.6
Sn2—C7—H7B109.5N6—C28—C27122.6 (12)
H7A—C7—H7B109.5N6—C28—H28118.7
Sn2—C7—H7C109.5C27—C28—H28118.7
Symmetry codes: (i) x+1, y, z1/2; (ii) x1, y, z+1/2.
 

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