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The structure determination of the deep-red centrosymmetric tin(IV) complex, [Sn(C48H36N4)(C10H7O)2], shows an octahedral Sn atom within a trans-N4O2 donor set.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801017214/tk6042sup1.cif
Contains datablocks k15_01, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801017214/tk6042Isup2.hkl
Contains datablock I

CCDC reference: 177176

Key indicators

  • Single-crystal X-ray study
  • T = 123 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.027
  • wR factor = 0.067
  • Data-to-parameter ratio = 18.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Computing details top

Data collection: COLLECT (Nonius, 1997-2000); cell refinement: HKL SCALEPACK (Otwinowski & Minor 1997); data reduction: HKL DENZO and SCALEPACK (Otwinowski & Minor 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

(I) top
Crystal data top
[Sn(C48H36N4)(C10H7O)2]Z = 1
Mr = 1073.9F(000) = 552
Triclinic, P1Dx = 1.380 Mg m3
a = 11.166 (1) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.409 (1) ÅCell parameters from 34660 reflections
c = 11.724 (1) Åθ = 2.8–28.3°
α = 107.63 (1)°µ = 0.55 mm1
β = 110.44 (1)°T = 123 K
γ = 96.68 (1)°Prism, red
V = 1291.9 (2) Å30.12 × 0.12 × 0.05 mm
Data collection top
KappaCCD
diffractometer
6153 reflections with I > 2σ(I)
CCD rotation images, thick slices scansRint = 0.037
Absorption correction: analytical
(Alcock, 1970)
θmax = 28.3°, θmin = 2.8°
Tmin = 0.898, Tmax = 0.953h = 1414
22917 measured reflectionsk = 1515
6331 independent reflectionsl = 1514
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.027 w = 1/[σ2(Fo2) + (0.0267P)2 + 0.91P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.067(Δ/σ)max = 0.001
S = 1.03Δρmax = 0.49 e Å3
6331 reflectionsΔρmin = 0.56 e Å3
342 parameters
Special details top

Experimental. 1H n.m.r. (300 MHz, CDCl3): δ 2.07 (s, 2H, H26), 2.19 (d,J8.7 Hz, 2H, H34), 2.72 (s, 12H, H17,24), 6.11 (d, J8.8 Hz, 2H, H33), 6.49, (d, J7.3 Hz, 2H, H28), 6.96 (m, 4H, H29,31), 7.14 (d, J7.3 Hz, 2H, H30), 7.52 (d, J7.9 Hz, 8H, H2,3,7,8), 7.79 (d, J7.9 Hz, 8H, H13,15,20,22), and 9.08 (s, 8H, H12,16,19,23).

13C n.m.r. (50 MHz, CDCl3): δ 21.86, 112.09, 120.89, 121.72, 122.17, 124.67, 125.62, 125.72, 126.89, 127.91, 132.72, 132.83, 133.54, 135.10, 138.29, 138.35, 147.76 and 152.76.

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sn10000.01824 (5)
N10.09294 (12)0.10571 (12)0.10760 (13)0.0201 (3)
N20.12224 (13)0.16941 (12)0.02873 (13)0.0200 (3)
O10.13203 (11)0.01015 (10)0.16897 (11)0.0253 (2)
C10.18972 (15)0.05450 (15)0.13833 (15)0.0216 (3)
C20.21889 (16)0.15798 (15)0.22235 (16)0.0243 (3)
C30.13951 (16)0.26798 (15)0.24093 (16)0.0244 (3)
C40.05931 (15)0.23559 (14)0.16845 (15)0.0207 (3)
C50.03783 (15)0.32111 (14)0.16307 (15)0.0208 (3)
C60.12194 (15)0.28994 (14)0.09942 (15)0.0208 (3)
C70.22343 (16)0.37823 (15)0.09692 (16)0.0245 (3)
C80.28174 (16)0.31009 (15)0.02499 (16)0.0247 (3)
C90.21879 (15)0.17767 (14)0.01794 (15)0.0209 (3)
C100.24979 (15)0.07532 (15)0.09571 (15)0.0216 (3)
C110.05453 (16)0.46024 (14)0.23231 (16)0.0221 (3)
C120.1434 (2)0.52376 (16)0.36134 (18)0.0320 (4)
C130.1598 (2)0.65334 (17)0.42211 (18)0.0341 (4)
C140.08899 (19)0.72151 (15)0.35643 (18)0.0295 (4)
C150.0016 (2)0.65816 (18)0.2284 (2)0.0388 (4)
C160.0161 (2)0.52828 (17)0.16602 (19)0.0354 (4)
C170.1071 (2)0.86245 (17)0.4217 (2)0.0438 (5)
C180.35719 (16)0.10843 (15)0.13811 (16)0.0230 (3)
C190.32736 (19)0.1090 (2)0.2624 (2)0.0357 (4)
C200.4269 (2)0.1375 (2)0.3027 (2)0.0411 (5)
C210.55772 (19)0.16866 (18)0.2186 (2)0.0339 (4)
C220.5874 (2)0.1689 (3)0.0949 (2)0.0490 (6)
C230.48863 (19)0.1394 (2)0.0539 (2)0.0450 (5)
C240.6658 (2)0.2015 (2)0.2615 (3)0.0489 (6)
C250.20922 (16)0.09525 (15)0.27362 (16)0.0235 (3)
C260.16602 (16)0.15453 (15)0.36735 (16)0.0236 (3)
C270.24725 (16)0.26581 (15)0.47652 (16)0.0245 (3)
C280.20355 (18)0.32917 (17)0.57366 (18)0.0305 (4)
C290.2843 (2)0.43609 (19)0.67819 (19)0.0393 (4)
C300.4115 (2)0.4865 (2)0.6906 (2)0.0451 (5)
C310.4566 (2)0.42819 (19)0.6007 (2)0.0390 (4)
C320.37654 (17)0.31603 (17)0.49018 (17)0.0289 (4)
C330.41992 (17)0.25144 (19)0.39411 (19)0.0330 (4)
C340.33944 (17)0.14439 (18)0.28950 (18)0.0296 (4)
H20.28230.15060.25830.029*
H30.13730.35120.29240.029*
H70.24560.4680.13820.029*
H80.35150.34370.00630.03*
H120.19330.47870.40840.038*
H130.2210.69580.51070.041*
H150.04770.70360.18140.047*
H160.07710.48630.07730.042*
H17A0.06740.89770.3550.066*
H17B0.20150.90410.46950.066*
H17C0.06430.87690.48310.066*
H190.23770.08970.32140.043*
H200.40420.13540.38940.049*
H220.67730.18950.03580.059*
H230.51180.14060.03260.054*
H24A0.68980.29350.23920.073*
H24B0.63450.15780.35640.073*
H24C0.74320.17460.21670.073*
H260.08020.12030.35870.028*
H280.11750.29680.56570.037*
H290.25430.47670.74290.047*
H300.4660.56190.76260.054*
H310.54320.46260.61140.047*
H330.50640.2830.40250.04*
H340.37090.10240.22670.035*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.01673 (8)0.01371 (7)0.02231 (8)0.00245 (5)0.00963 (6)0.00252 (5)
N10.0182 (6)0.0158 (6)0.0248 (7)0.0040 (5)0.0109 (5)0.0029 (5)
N20.0193 (6)0.0152 (6)0.0243 (7)0.0026 (5)0.0108 (5)0.0039 (5)
O10.0261 (6)0.0176 (5)0.0252 (6)0.0051 (4)0.0061 (5)0.0042 (4)
C10.0195 (7)0.0212 (7)0.0239 (8)0.0054 (6)0.0113 (6)0.0049 (6)
C20.0257 (8)0.0213 (7)0.0278 (8)0.0073 (6)0.0158 (7)0.0054 (6)
C30.0276 (8)0.0190 (7)0.0274 (8)0.0074 (6)0.0149 (7)0.0045 (6)
C40.0219 (7)0.0169 (7)0.0224 (8)0.0064 (6)0.0098 (6)0.0043 (6)
C50.0230 (7)0.0155 (7)0.0215 (7)0.0047 (6)0.0086 (6)0.0041 (6)
C60.0213 (7)0.0147 (7)0.0226 (8)0.0024 (6)0.0079 (6)0.0039 (6)
C70.0259 (8)0.0164 (7)0.0285 (8)0.0013 (6)0.0124 (7)0.0045 (6)
C80.0233 (8)0.0192 (7)0.0290 (8)0.0002 (6)0.0123 (7)0.0055 (6)
C90.0184 (7)0.0187 (7)0.0233 (8)0.0019 (6)0.0090 (6)0.0053 (6)
C100.0181 (7)0.0213 (7)0.0240 (8)0.0037 (6)0.0098 (6)0.0056 (6)
C110.0257 (8)0.0155 (7)0.0265 (8)0.0043 (6)0.0148 (6)0.0050 (6)
C120.0448 (10)0.0207 (8)0.0276 (9)0.0094 (7)0.0125 (8)0.0071 (7)
C130.0461 (11)0.0215 (8)0.0280 (9)0.0035 (7)0.0154 (8)0.0018 (7)
C140.0394 (10)0.0167 (7)0.0411 (10)0.0056 (7)0.0287 (8)0.0084 (7)
C150.0483 (12)0.0250 (9)0.0445 (11)0.0170 (8)0.0164 (9)0.0145 (8)
C160.0403 (10)0.0246 (9)0.0321 (10)0.0116 (8)0.0070 (8)0.0061 (7)
C170.0624 (14)0.0178 (8)0.0592 (13)0.0081 (9)0.0387 (11)0.0092 (8)
C180.0212 (7)0.0182 (7)0.0298 (8)0.0038 (6)0.0137 (6)0.0054 (6)
C190.0267 (9)0.0466 (11)0.0421 (11)0.0087 (8)0.0150 (8)0.0265 (9)
C200.0378 (10)0.0564 (13)0.0500 (12)0.0165 (9)0.0247 (9)0.0376 (11)
C210.0338 (9)0.0314 (9)0.0554 (12)0.0151 (8)0.0299 (9)0.0247 (9)
C220.0208 (9)0.0813 (17)0.0484 (13)0.0085 (10)0.0154 (9)0.0282 (12)
C230.0239 (9)0.0787 (16)0.0320 (10)0.0060 (10)0.0124 (8)0.0210 (10)
C240.0424 (12)0.0581 (14)0.0836 (17)0.0251 (10)0.0452 (12)0.0479 (13)
C250.0227 (7)0.0186 (7)0.0249 (8)0.0039 (6)0.0059 (6)0.0075 (6)
C260.0203 (7)0.0212 (7)0.0280 (8)0.0024 (6)0.0085 (6)0.0098 (6)
C270.0263 (8)0.0204 (7)0.0248 (8)0.0046 (6)0.0085 (6)0.0086 (6)
C280.0314 (9)0.0281 (9)0.0320 (9)0.0066 (7)0.0129 (7)0.0113 (7)
C290.0524 (12)0.0316 (10)0.0293 (10)0.0117 (9)0.0162 (9)0.0049 (8)
C300.0504 (12)0.0298 (10)0.0317 (10)0.0038 (9)0.0045 (9)0.0005 (8)
C310.0306 (9)0.0338 (10)0.0371 (11)0.0078 (8)0.0045 (8)0.0088 (8)
C320.0269 (8)0.0256 (8)0.0288 (9)0.0002 (7)0.0071 (7)0.0101 (7)
C330.0210 (8)0.0388 (10)0.0360 (10)0.0004 (7)0.0104 (7)0.0137 (8)
C340.0250 (8)0.0339 (9)0.0298 (9)0.0076 (7)0.0125 (7)0.0099 (7)
Geometric parameters (Å, º) top
Sn1—O1i2.0616 (12)C22—C231.394 (3)
Sn1—O12.0616 (12)C25—C261.376 (2)
Sn1—N2i2.0936 (13)C25—C341.422 (2)
Sn1—N22.0936 (13)C26—C271.418 (2)
Sn1—N1i2.0993 (12)C27—C321.424 (2)
Sn1—N12.0993 (12)C27—C281.424 (2)
N1—C41.3743 (19)C28—C291.367 (3)
N1—C11.375 (2)C29—C301.409 (3)
N2—C91.3748 (19)C30—C311.353 (3)
N2—C61.3749 (19)C31—C321.427 (3)
O1—C251.3494 (19)C32—C331.417 (3)
C1—C10i1.407 (2)C33—C341.368 (3)
C1—C21.442 (2)C2—H20.95
C2—C31.360 (2)C3—H30.95
C3—C41.442 (2)C7—H70.95
C4—C51.404 (2)C8—H80.95
C5—C61.404 (2)C12—H120.95
C5—C111.503 (2)C13—H130.95
C6—C71.441 (2)C15—H150.95
C7—C81.358 (2)C16—H160.95
C8—C91.441 (2)C17—H17A0.98
C9—C101.409 (2)C17—H17B0.98
C10—C1i1.407 (2)C17—H17C0.98
C10—C181.501 (2)C19—H190.95
C11—C161.381 (2)C20—H200.95
C11—C121.385 (2)C22—H220.95
C12—C131.391 (2)C23—H230.95
C13—C141.380 (3)C24—H24A0.98
C14—C151.372 (3)C24—H24B0.98
C14—C171.511 (2)C24—H24C0.98
C15—C161.394 (3)C26—H260.95
C18—C191.380 (3)C28—H280.95
C18—C231.382 (3)C29—H290.95
C19—C201.392 (3)C30—H300.95
C20—C211.376 (3)C31—H310.95
C21—C221.369 (3)C33—H330.95
C21—C241.511 (2)C34—H340.95
O1i—Sn1—O1180.00 (9)O1—C25—C34119.37 (15)
O1i—Sn1—N2i91.63 (5)C26—C25—C34119.12 (15)
O1—Sn1—N2i88.37 (5)C25—C26—C27121.19 (15)
O1i—Sn1—N288.37 (5)C26—C27—C32119.31 (15)
O1—Sn1—N291.63 (5)C26—C27—C28121.92 (15)
N2i—Sn1—N2180.00 (8)C32—C27—C28118.76 (15)
O1i—Sn1—N1i90.03 (5)C29—C28—C27120.64 (18)
O1—Sn1—N1i89.97 (5)C28—C29—C30120.50 (19)
N2i—Sn1—N1i89.47 (5)C31—C30—C29120.41 (18)
N2—Sn1—N1i90.53 (5)C30—C31—C32121.30 (19)
O1i—Sn1—N189.97 (5)C33—C32—C27118.41 (16)
O1—Sn1—N190.03 (5)C33—C32—C31123.22 (17)
N2i—Sn1—N190.53 (5)C27—C32—C31118.37 (17)
N2—Sn1—N189.47 (5)C34—C33—C32121.12 (16)
N1i—Sn1—N1180.00 (10)C33—C34—C25120.81 (16)
C4—N1—C1109.03 (12)C3—C2—H2126.1
C4—N1—Sn1125.86 (10)C1—C2—H2126.1
C1—N1—Sn1124.87 (10)C2—C3—H3126.2
C9—N2—C6108.78 (12)C4—C3—H3126.2
C9—N2—Sn1125.14 (10)C8—C7—H7126.1
C6—N2—Sn1126.07 (10)C6—C7—H7126.1
C25—O1—Sn1121.68 (10)C7—C8—H8126.1
N1—C1—C10i126.37 (14)C9—C8—H8126.1
N1—C1—C2107.66 (13)C11—C12—H12119.9
C10i—C1—C2125.98 (14)C13—C12—H12119.9
C3—C2—C1107.85 (14)C14—C13—H13119.3
C2—C3—C4107.65 (14)C12—C13—H13119.3
N1—C4—C5125.99 (14)C14—C15—H15119.4
N1—C4—C3107.81 (13)C16—C15—H15119.4
C5—C4—C3126.18 (14)C11—C16—H16119.8
C4—C5—C6126.55 (14)C15—C16—H16119.8
C4—C5—C11117.23 (13)C14—C17—H17A109.5
C6—C5—C11116.22 (14)C14—C17—H17B109.5
N2—C6—C5125.95 (14)H17A—C17—H17B109.5
N2—C6—C7107.86 (13)C14—C17—H17C109.5
C5—C6—C7126.19 (14)H17A—C17—H17C109.5
C8—C7—C6107.76 (14)H17B—C17—H17C109.5
C7—C8—C9107.72 (14)C18—C19—H19119.5
N2—C9—C10126.31 (14)C20—C19—H19119.5
N2—C9—C8107.89 (13)C21—C20—H20119.5
C10—C9—C8125.80 (14)C19—C20—H20119.5
C1i—C10—C9126.63 (14)C21—C22—H22119.3
C1i—C10—C18116.80 (14)C23—C22—H22119.3
C9—C10—C18116.57 (14)C18—C23—H23119.8
C16—C11—C12118.67 (15)C22—C23—H23119.8
C16—C11—C5120.07 (15)C21—C24—H24A109.5
C12—C11—C5121.22 (15)C21—C24—H24B109.5
C11—C12—C13120.13 (17)H24A—C24—H24B109.5
C14—C13—C12121.37 (18)C21—C24—H24C109.5
C15—C14—C13118.21 (16)H24A—C24—H24C109.5
C15—C14—C17120.23 (18)H24B—C24—H24C109.5
C13—C14—C17121.55 (18)C25—C26—H26119.4
C14—C15—C16121.16 (18)C27—C26—H26119.4
C11—C16—C15120.46 (18)C29—C28—H28119.7
C19—C18—C23118.08 (16)C27—C28—H28119.7
C19—C18—C10120.85 (15)C28—C29—H29119.8
C23—C18—C10121.07 (16)C30—C29—H29119.7
C18—C19—C20120.92 (18)C31—C30—H30119.8
C21—C20—C19120.91 (19)C29—C30—H30119.8
C22—C21—C20118.21 (17)C30—C31—H31119.3
C22—C21—C24120.83 (19)C32—C31—H31119.3
C20—C21—C24120.96 (19)C34—C33—H33119.4
C21—C22—C23121.38 (19)C32—C33—H33119.4
C18—C23—C22120.49 (19)C33—C34—H34119.6
O1—C25—C26121.49 (15)C25—C34—H34119.6
Symmetry code: (i) x, y, z.
 

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