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The trinuclear title compound, (μ2-dppf){Cd(S2CNEt2)2}2 or [Cd2Fe(C3H10NS2)4(C21H14P)2], is disposed about a crystallographic centre of inversion and features five-coordinate Cd atoms that exist in distorted square-pyramidal geometries defined by a PS4 donor set.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802003604/ww6010sup1.cif
Contains datablocks general, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802003604/ww6010Isup2.hkl
Contains datablock I

CCDC reference: 183760

Key indicators

  • Single-crystal X-ray study
  • T = 223 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.031
  • wR factor = 0.074
  • Data-to-parameter ratio = 27.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SHELXTL (Bruker, 2000); program(s) used to solve structure: DIRDIF92 PATTY (Beurskens et al., 1992); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
C54H68Cd2FeN4P2S8F(000) = 2800
Mr = 1372.19Dx = 1.510 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2ycCell parameters from 24873 reflections
a = 16.6641 (6) Åθ = 1.5–30.1°
b = 13.1396 (5) ŵ = 1.30 mm1
c = 27.8664 (11) ÅT = 223 K
β = 98.482 (1)°Block, pale-yellow
V = 6034.9 (4) Å30.42 × 0.23 × 0.23 mm
Z = 4
Data collection top
Bruker AXS SMART CCD
diffractometer
8787 independent reflections
Radiation source: fine-focus sealed tube7066 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
ω scansθmax = 30.1°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 2314
Tmin = 0.573, Tmax = 0.741k = 1718
24873 measured reflectionsl = 3739
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)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.074H-atom parameters constrained
S = 0.95 w = 1/[σ2(Fo2) + (0.0404P)2]
where P = (Fo2 + 2Fc2)/3
8787 reflections(Δ/σ)max = 0.001
323 parametersΔρmax = 0.71 e Å3
0 restraintsΔρmin = 0.32 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*/Ueq
Cd0.214866 (8)0.034561 (11)0.127986 (5)0.03017 (5)
Fe0.25000.25000.00000.02823 (9)
S10.23792 (3)0.14740 (4)0.095223 (18)0.03608 (12)
S20.10837 (3)0.00617 (4)0.05161 (2)0.03971 (13)
S30.12781 (3)0.14280 (5)0.17920 (2)0.03962 (12)
S40.27831 (3)0.03239 (4)0.220067 (18)0.03501 (11)
P10.33957 (3)0.13779 (4)0.103487 (17)0.02560 (10)
N10.12928 (10)0.19157 (12)0.01805 (6)0.0319 (3)
N20.21166 (10)0.17880 (13)0.26649 (6)0.0344 (4)
C10.15553 (11)0.12256 (14)0.05151 (7)0.0276 (4)
C20.06287 (13)0.16968 (18)0.02157 (8)0.0437 (5)
H2a0.02520.12120.01010.0606 (14)*
H2b0.03290.23260.03080.0606 (14)*
C30.09371 (17)0.1262 (3)0.06539 (9)0.0705 (9)
H3a0.04830.11330.09070.0727 (16)*
H3b0.13050.17430.07710.0727 (16)*
H3c0.12220.06290.05660.0727 (16)*
C40.16098 (13)0.29614 (15)0.01951 (8)0.0372 (4)
H4a0.21750.29630.03540.0606 (14)*
H4b0.16000.32120.01370.0606 (14)*
C50.11155 (17)0.36621 (18)0.04653 (10)0.0559 (7)
H5a0.13410.43430.04710.0727 (16)*
H5b0.05590.36740.03030.0727 (16)*
H5c0.11290.34190.07950.0727 (16)*
C60.20633 (11)0.12390 (14)0.22640 (7)0.0296 (4)
C70.27885 (14)0.16568 (18)0.30685 (7)0.0431 (5)
H7a0.29610.09430.30850.0606 (14)*
H7b0.25980.18270.33750.0606 (14)*
C80.35024 (15)0.2324 (2)0.30057 (10)0.0579 (7)
H8a0.39340.22170.32750.0727 (16)*
H8b0.33360.30320.29970.0727 (16)*
H8c0.36960.21510.27040.0727 (16)*
C90.15626 (14)0.26379 (17)0.27244 (8)0.0442 (5)
H9a0.13070.28680.24030.0606 (14)*
H9b0.18770.32070.28820.0606 (14)*
C100.09164 (16)0.2353 (2)0.30181 (11)0.0631 (7)
H10a0.05690.29360.30460.0727 (16)*
H10b0.11650.21410.33390.0727 (16)*
H10c0.05960.17980.28600.0727 (16)*
C110.33543 (11)0.16171 (14)0.03954 (7)0.0281 (4)
C120.28745 (11)0.10210 (15)0.00344 (7)0.0312 (4)
H120.25590.04530.00910.0485 (11)*
C130.29550 (14)0.14331 (17)0.04255 (7)0.0401 (5)
H130.27030.11830.07270.0485 (11)*
C140.34752 (13)0.22784 (18)0.03557 (8)0.0414 (5)
H140.36280.26920.06020.0485 (11)*
C150.37313 (11)0.24022 (16)0.01491 (8)0.0358 (4)
H150.40840.29080.02960.0485 (11)*
C160.36928 (12)0.25703 (14)0.13385 (7)0.0322 (4)
C170.44381 (14)0.30290 (16)0.13093 (9)0.0462 (5)
H170.48000.27230.11240.0485 (11)*
C180.46491 (18)0.3928 (2)0.15502 (12)0.0659 (8)
H180.51490.42390.15260.0485 (11)*
C190.4127 (2)0.4367 (2)0.18256 (12)0.0751 (9)
H190.42760.49740.19950.0485 (11)*
C200.3386 (2)0.3930 (2)0.18574 (10)0.0657 (8)
H200.30300.42420.20450.0485 (11)*
C210.31637 (15)0.30330 (16)0.16145 (8)0.0440 (5)
H210.26570.27360.16360.0485 (11)*
C220.42824 (11)0.05673 (14)0.11904 (7)0.0278 (4)
C230.45219 (13)0.00965 (16)0.08529 (8)0.0376 (5)
H230.42440.01040.05340.0485 (11)*
C240.51713 (14)0.07522 (17)0.09837 (9)0.0468 (6)
H240.53310.12010.07530.0485 (11)*
C250.55817 (13)0.07481 (17)0.14505 (10)0.0468 (6)
H250.60230.11900.15370.0485 (11)*
C260.53476 (14)0.01024 (19)0.17883 (9)0.0479 (6)
H260.56280.01010.21070.0485 (11)*
C270.46940 (13)0.05540 (17)0.16620 (8)0.0393 (5)
H270.45310.09900.18970.0485 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd0.03295 (8)0.03153 (8)0.02601 (7)0.00076 (5)0.00432 (5)0.00295 (5)
Fe0.0303 (2)0.0310 (2)0.02509 (18)0.01250 (15)0.00959 (15)0.00529 (15)
S10.0473 (3)0.0300 (2)0.0284 (2)0.0086 (2)0.0028 (2)0.00077 (19)
S20.0369 (3)0.0331 (3)0.0452 (3)0.0080 (2)0.0069 (2)0.0086 (2)
S30.0325 (3)0.0519 (3)0.0338 (3)0.0094 (2)0.0029 (2)0.0060 (2)
S40.0436 (3)0.0346 (3)0.0259 (2)0.0113 (2)0.0021 (2)0.00141 (19)
P10.0262 (2)0.0253 (2)0.0253 (2)0.00427 (17)0.00366 (17)0.00084 (18)
N10.0314 (8)0.0313 (8)0.0326 (8)0.0018 (6)0.0040 (7)0.0041 (7)
N20.0400 (9)0.0335 (9)0.0300 (8)0.0027 (7)0.0058 (7)0.0049 (7)
C10.0292 (9)0.0273 (9)0.0275 (9)0.0017 (7)0.0081 (7)0.0004 (7)
C20.0324 (11)0.0482 (13)0.0467 (13)0.0012 (9)0.0063 (9)0.0146 (10)
C30.0634 (18)0.110 (3)0.0353 (13)0.0269 (16)0.0023 (12)0.0031 (15)
C40.0431 (12)0.0304 (10)0.0395 (11)0.0005 (8)0.0109 (9)0.0088 (8)
C50.0726 (18)0.0346 (12)0.0655 (17)0.0045 (11)0.0266 (14)0.0018 (11)
C60.0335 (10)0.0284 (9)0.0282 (9)0.0007 (7)0.0083 (7)0.0014 (7)
C70.0531 (13)0.0471 (13)0.0273 (10)0.0033 (10)0.0003 (9)0.0090 (9)
C80.0513 (15)0.0626 (17)0.0561 (16)0.0060 (12)0.0040 (12)0.0105 (13)
C90.0572 (14)0.0338 (11)0.0418 (12)0.0041 (10)0.0077 (10)0.0062 (9)
C100.0580 (17)0.0684 (18)0.0671 (18)0.0151 (13)0.0233 (14)0.0014 (14)
C110.0284 (9)0.0294 (9)0.0272 (9)0.0092 (7)0.0068 (7)0.0037 (7)
C120.0331 (10)0.0321 (10)0.0286 (9)0.0121 (8)0.0056 (8)0.0013 (7)
C130.0483 (12)0.0467 (12)0.0264 (10)0.0251 (10)0.0094 (9)0.0014 (9)
C140.0413 (12)0.0506 (13)0.0368 (11)0.0235 (10)0.0204 (9)0.0159 (10)
C150.0284 (10)0.0398 (11)0.0417 (11)0.0101 (8)0.0135 (8)0.0097 (9)
C160.0379 (11)0.0255 (9)0.0313 (10)0.0055 (8)0.0007 (8)0.0002 (7)
C170.0399 (12)0.0335 (11)0.0621 (15)0.0004 (9)0.0024 (10)0.0030 (10)
C180.0681 (18)0.0390 (14)0.084 (2)0.0117 (12)0.0098 (16)0.0020 (14)
C190.120 (3)0.0306 (13)0.069 (2)0.0041 (16)0.0057 (19)0.0146 (13)
C200.112 (3)0.0373 (13)0.0512 (16)0.0147 (15)0.0232 (16)0.0082 (12)
C210.0639 (15)0.0326 (11)0.0375 (11)0.0097 (10)0.0141 (10)0.0005 (9)
C220.0231 (9)0.0255 (9)0.0347 (10)0.0022 (7)0.0039 (7)0.0035 (7)
C230.0348 (11)0.0352 (11)0.0418 (12)0.0078 (8)0.0017 (9)0.0038 (9)
C240.0413 (12)0.0346 (11)0.0655 (16)0.0120 (9)0.0106 (11)0.0020 (11)
C250.0301 (11)0.0357 (11)0.0723 (17)0.0096 (9)0.0000 (10)0.0132 (11)
C260.0401 (12)0.0499 (14)0.0483 (13)0.0067 (10)0.0114 (10)0.0109 (11)
C270.0389 (12)0.0404 (12)0.0366 (11)0.0075 (9)0.0010 (9)0.0014 (9)
Geometric parameters (Å, º) top
Cd—S12.6079 (5)C8—H8B0.9700
Cd—S22.6175 (5)C8—H8C0.9700
Cd—S32.6029 (5)C9—C101.493 (3)
Cd—S42.6273 (5)C9—H9A0.9800
Cd—P12.6539 (5)C9—H9B0.9800
Fe—C112.0308 (17)C10—H10A0.9700
Fe—C122.0390 (18)C10—H10B0.9700
Fe—C142.0453 (19)C10—H10C0.9700
Fe—C152.0366 (19)C11—C151.434 (3)
Fe—C132.0521 (19)C11—C121.424 (3)
S1—C11.7269 (19)C12—C131.416 (3)
S2—C11.7196 (19)C12—H120.9400
S3—C61.7310 (19)C13—C141.405 (3)
S4—C61.7257 (19)C13—H130.9400
P1—C111.8006 (19)C14—C151.418 (3)
P1—C161.8144 (19)C14—H140.9400
P1—C221.8212 (18)C15—H150.9400
N1—C11.328 (2)C16—C211.392 (3)
N1—C41.470 (2)C16—C171.394 (3)
N1—C21.472 (3)C17—C181.379 (3)
N2—C61.322 (2)C17—H170.9400
N2—C91.474 (3)C18—C191.369 (5)
N2—C71.475 (3)C18—H180.9400
C2—C31.506 (4)C19—C201.377 (4)
C2—H2A0.9800C19—H190.9400
C2—H2B0.9800C20—C211.382 (3)
C3—H3A0.9700C20—H200.9400
C3—H3B0.9700C21—H210.9400
C3—H3C0.9700C22—C231.384 (3)
C4—C51.509 (3)C22—C271.390 (3)
C4—H4A0.9800C23—C241.389 (3)
C4—H4B0.9800C23—H230.9400
C5—H5A0.9700C24—C251.378 (3)
C5—H5B0.9700C24—H240.9400
C5—H5C0.9700C25—C261.366 (4)
C7—C81.508 (3)C25—H250.9400
C7—H7A0.9800C26—C271.393 (3)
C7—H7B0.9800C26—H260.9400
C8—H8A0.9700C27—H270.9400
S1—Cd—S269.213 (16)N2—C7—C8111.5 (2)
S1—Cd—S3144.657 (19)N2—C7—H7A109.3
S1—Cd—S4105.851 (16)C8—C7—H7A109.3
S2—Cd—S3101.051 (17)N2—C7—H7B109.3
S2—Cd—S4156.76 (2)C8—C7—H7B109.3
S3—Cd—S469.328 (16)H7A—C7—H7B108.0
S1—Cd—P1102.541 (17)C7—C8—H8A109.5
S2—Cd—P1110.979 (18)C7—C8—H8B109.5
S3—Cd—P1112.501 (18)H8A—C8—H8B109.5
S4—Cd—P192.246 (17)C7—C8—H8C109.5
C11—Fe—C11i180.00 (9)H8A—C8—H8C109.5
C11—Fe—C1240.96 (7)H8B—C8—H8C109.5
C11i—Fe—C12139.04 (7)N2—C9—C10112.7 (2)
C11—Fe—C12i139.04 (7)N2—C9—H9A109.0
C12—Fe—C12i180.0C10—C9—H9A109.0
C11—Fe—C1468.78 (8)N2—C9—H9B109.0
C11i—Fe—C14111.21 (8)C10—C9—H9B109.0
C12—Fe—C1468.13 (8)H9A—C9—H9B107.8
C12i—Fe—C14111.87 (8)C9—C10—H10A109.5
C11—Fe—C14i111.21 (8)C9—C10—H10B109.5
C12—Fe—C14i111.87 (8)H10A—C10—H10B109.5
C14—Fe—C14i180.00 (10)C9—C10—H10C109.5
C11—Fe—C15i138.70 (8)H10A—C10—H10C109.5
C12—Fe—C15i111.22 (8)H10B—C10—H10C109.5
C14—Fe—C15i139.35 (8)C15—C11—C12107.30 (17)
C11—Fe—C1541.30 (8)C15—C11—P1130.05 (16)
C11i—Fe—C15138.70 (8)C12—C11—P1122.61 (15)
C12—Fe—C1568.78 (8)C15—C11—Fe69.57 (10)
C12i—Fe—C15111.22 (8)C12—C11—Fe69.83 (10)
C14—Fe—C1540.65 (8)P1—C11—Fe123.93 (9)
C14i—Fe—C15139.35 (8)C13—C12—C11108.12 (19)
C15i—Fe—C15180.0C13—C12—Fe70.26 (11)
C11—Fe—C1368.54 (8)C11—C12—Fe69.21 (10)
C11i—Fe—C13111.46 (8)C13—C12—H12125.9
C12—Fe—C1340.49 (8)C11—C12—H12125.9
C12i—Fe—C13139.51 (8)Fe—C12—H12126.2
C14—Fe—C1340.10 (9)C14—C13—C12108.42 (19)
C14i—Fe—C13139.90 (9)C14—C13—Fe69.69 (12)
C15i—Fe—C13111.85 (9)C12—C13—Fe69.26 (11)
C15—Fe—C1368.15 (9)C14—C13—H13125.8
C11—Fe—C13i111.46 (8)C12—C13—H13125.8
C12—Fe—C13i139.51 (8)Fe—C13—H13126.8
C14—Fe—C13i139.90 (9)C13—C14—C15108.51 (18)
C15—Fe—C13i111.85 (9)C13—C14—Fe70.21 (12)
C13—Fe—C13i180.00 (13)C15—C14—Fe69.35 (11)
Cd—S1—C186.03 (6)C13—C14—H14125.7
Cd—S2—C185.87 (6)C15—C14—H14125.7
Cd—S3—C685.31 (6)Fe—C14—H14126.3
Cd—S4—C684.65 (6)C11—C15—C14107.65 (19)
C16—P1—C11106.19 (9)C11—C15—Fe69.13 (10)
C16—P1—C22103.77 (9)C14—C15—Fe70.00 (11)
C11—P1—C22104.41 (8)C11—C15—H15126.2
C16—P1—Cd119.44 (7)C14—C15—H15126.2
C11—P1—Cd115.25 (6)Fe—C15—H15126.3
C22—P1—Cd106.17 (6)C21—C16—C17119.1 (2)
C1—N1—C4122.61 (16)C21—C16—P1118.90 (16)
C1—N1—C2121.78 (17)C17—C16—P1122.03 (16)
C4—N1—C2115.52 (16)C18—C17—C16120.5 (2)
C6—N2—C9122.92 (17)C18—C17—H17119.7
C6—N2—C7121.96 (17)C16—C17—H17119.7
C9—N2—C7114.85 (16)C17—C18—C19119.8 (3)
S1—C1—S2118.88 (11)C17—C18—H18120.1
S1—C1—N1120.77 (14)C19—C18—H18120.1
S2—C1—N1120.35 (14)C20—C19—C18120.7 (3)
N1—C2—C3111.95 (19)C20—C19—H19119.7
N1—C2—H2A109.2C18—C19—H19119.7
C3—C2—H2A109.2C21—C20—C19120.2 (3)
N1—C2—H2B109.2C21—C20—H20119.9
C3—C2—H2B109.2C19—C20—H20119.9
H2A—C2—H2B107.9C20—C21—C16119.8 (2)
C2—C3—H3A109.5C20—C21—H21120.1
C2—C3—H3B109.5C16—C21—H21120.1
H3A—C3—H3B109.5C23—C22—C27118.88 (18)
C2—C3—H3C109.5C23—C22—P1120.80 (15)
H3A—C3—H3C109.5C27—C22—P1120.15 (15)
H3B—C3—H3C109.5C22—C23—C24120.3 (2)
N1—C4—C5111.33 (17)C22—C23—H23119.9
N1—C4—H4A109.4C24—C23—H23119.9
C5—C4—H4A109.4C25—C24—C23120.3 (2)
N1—C4—H4B109.4C25—C24—H24119.9
C5—C4—H4B109.4C23—C24—H24119.9
H4A—C4—H4B108.0C26—C25—C24120.0 (2)
C4—C5—H5A109.5C26—C25—H25120.0
C4—C5—H5B109.5C24—C25—H25120.0
H5A—C5—H5B109.5C25—C26—C27120.2 (2)
C4—C5—H5C109.5C25—C26—H26119.9
H5A—C5—H5C109.5C27—C26—H26119.9
H5B—C5—H5C109.5C22—C27—C26120.3 (2)
S3—C6—S4118.76 (11)C22—C27—H27119.8
S3—C6—N2120.86 (15)C26—C27—H27119.8
S4—C6—N2120.38 (15)
Symmetry code: (i) x+1/2, y+1/2, z.
 

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