[1,2-Bis(diphenyl­phosphino)ethane]bis­(N,N-dimethyl­dithio­carbamato)iron(III) tetra­fluoro­borate

The title compound, [Fe(C₃H₆NS₂)₂(C₂₆H₂₄P₂)]BF₄, contains a six-coordinate iron(III) cationic complex, with two bidentate dimethyl­dithio­carbamate and one 1,2-bis­(diphenyl­phos­phino)ethane ligands, and a disordered tetra­fluoro­borate anion. The cation possesses a crystallographic twofold rotation axis. The cations assemble in the crystal structure in two-dimensional layers via complementary C—H...π(phen­yl) inter­actions with channels occupied by tetra­fluorborate anions.

Key indicators

• Single-crystal X-ray study
• T = 203 K
• Mean [sigma](C-C) = 0.006 Å
• Disorder in solvent or counterion
• R factor = 0.041
• wR factor = 0.130
• Data-to-parameter ratio = 17.6

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT141_ALERT_4_C su on a - Axis Small or Missing (x 100000) .....         10 Ang.
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.00 Ratio
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for          B
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      50.00 Perc.
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.26 Ratio
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      42.50 Deg.
              F4   -F1   -B       2.655   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      37.60 Deg.
              B    -F4   -F4      1.555   1.555   2.655
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      36.90 Deg.
              B    -F2   -F4      1.555   1.555   2.655
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      43.10 Deg.
              F4   -B    -F1      2.655   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      28.80 Deg.
              F4   -B    -B       1.555   1.555   2.655

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  10 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   6 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   4 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT; 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).

[1,2-Bis(diphenylphosphino)ethane]bis(N,N-dimethyldithiocarbamato)iron(III) tetrafluoroborate

Crystal data

[Fe(C3H6NS2)2(C26H24P2)]BF4	F(000) = 1612
Mr = 781.47	Dx = 1.421 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 15.5061 (1) Å	Cell parameters from 8192 reflections
b = 18.0353 (2) Å	θ = 1.8–27.5°
c = 13.5470 (2) Å	µ = 0.78 mm^−1
β = 105.337 (1)°	T = 203 K
V = 3653.59 (7) Å^3	Block, red
Z = 4	0.38 × 0.33 × 0.18 mm

Data collection

Siemens SMART CCD diffractometer	4038 independent reflections
Radiation source: fine-focus sealed tube	3496 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.017
Area–detector ω scans	θmax = 27.5°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −19→19
Tmin = 0.757, Tmax = 0.873	k = 0→23
10961 measured reflections	l = 0→17

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.130	H-atom parameters constrained
S = 0.89	w = 1/[σ^2(Fo^2) + (0.0678P)^2 + 17.7249P] where P = (Fo^2 + 2Fc^2)/3
4038 reflections	(Δ/σ)max = 0.001
230 parameters	Δρmax = 0.83 e Å^−3
4 restraints	Δρmin = −0.57 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Fe	0.5000	0.59683 (3)	0.2500	0.02609 (15)
P1	0.57619 (5)	0.69096 (4)	0.19435 (5)	0.02843 (17)
S1	0.59902 (5)	0.51599 (4)	0.21126 (6)	0.03629 (19)
S2	0.60539 (5)	0.57899 (4)	0.40406 (5)	0.03720 (19)
N	0.7325 (2)	0.48497 (19)	0.3780 (3)	0.0577 (8)
C1	0.5186 (2)	0.77855 (17)	0.2030 (3)	0.0425 (7)
H1A	0.5604	0.8199	0.2076	0.051*
H1B	0.4695	0.7854	0.1410	0.051*
C2	0.6579 (2)	0.52135 (18)	0.3382 (3)	0.0402 (7)
C3	0.7712 (3)	0.4362 (3)	0.3137 (4)	0.0839 (16)
H3A	0.7708	0.3854	0.3370	0.126*
H3B	0.8322	0.4514	0.3187	0.126*
H3C	0.7360	0.4398	0.2431	0.126*
C5	0.7786 (4)	0.4920 (4)	0.4862 (4)	0.0913 (18)
H5A	0.7356	0.4882	0.5265	0.137*
H5B	0.8083	0.5397	0.4985	0.137*
H5C	0.8226	0.4528	0.5058	0.137*
C11	0.58618 (18)	0.69253 (16)	0.0630 (2)	0.0304 (5)
C12	0.6192 (3)	0.7564 (2)	0.0290 (3)	0.0554 (10)
H12A	0.6375	0.7962	0.0744	0.066*
C13	0.6256 (3)	0.7623 (2)	−0.0708 (3)	0.0621 (11)
H13A	0.6480	0.8059	−0.0928	0.075*
C14	0.5991 (2)	0.7042 (2)	−0.1374 (2)	0.0445 (7)
H14A	0.6038	0.7078	−0.2050	0.053*
C15	0.5659 (2)	0.64082 (19)	−0.1054 (2)	0.0448 (7)
H15A	0.5470	0.6015	−0.1516	0.054*
C16	0.5597 (2)	0.63418 (17)	−0.0049 (2)	0.0386 (7)
H16A	0.5377	0.5902	0.0167	0.046*
C21	0.6916 (2)	0.70455 (18)	0.2686 (2)	0.0383 (7)
C22	0.7575 (2)	0.6561 (2)	0.2544 (3)	0.0464 (8)
H22A	0.7420	0.6189	0.2041	0.056*
C23	0.8460 (3)	0.6619 (3)	0.3136 (3)	0.0648 (12)
H23A	0.8897	0.6284	0.3044	0.078*
C24	0.8681 (3)	0.7178 (4)	0.3861 (3)	0.0823 (17)
H24A	0.9273	0.7223	0.4267	0.099*
C25	0.8044 (4)	0.7667 (3)	0.3992 (3)	0.0821 (17)
H25A	0.8205	0.8050	0.4476	0.099*
C26	0.7162 (3)	0.7602 (2)	0.3416 (3)	0.0602 (11)
H26A	0.6730	0.7936	0.3520	0.072*
F1	0.5807 (5)	0.9377 (4)	0.3099 (7)	0.091 (2)	0.50
F4	0.4527 (8)	0.9768 (9)	0.2241 (7)	0.163 (5)	0.50
F3	0.4864 (4)	0.9509 (6)	0.4095 (8)	0.188 (6)	0.50
F2	0.5431 (7)	1.0522 (4)	0.3186 (9)	0.163 (4)	0.50
B	0.5121 (10)	0.9801 (7)	0.3202 (11)	0.100 (5)*	0.50

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe	0.0311 (3)	0.0237 (3)	0.0249 (3)	0.000	0.0097 (2)	0.000
P1	0.0355 (4)	0.0275 (3)	0.0246 (3)	−0.0037 (3)	0.0120 (3)	−0.0020 (2)
S1	0.0429 (4)	0.0309 (4)	0.0387 (4)	0.0064 (3)	0.0172 (3)	0.0009 (3)
S2	0.0422 (4)	0.0386 (4)	0.0293 (4)	0.0024 (3)	0.0068 (3)	0.0034 (3)
N	0.0483 (17)	0.065 (2)	0.0578 (19)	0.0211 (15)	0.0105 (14)	0.0185 (16)
C1	0.063 (2)	0.0289 (14)	0.0459 (18)	0.0016 (14)	0.0328 (16)	0.0023 (12)
C2	0.0390 (16)	0.0388 (16)	0.0443 (17)	0.0075 (13)	0.0133 (13)	0.0125 (13)
C3	0.071 (3)	0.095 (4)	0.094 (4)	0.052 (3)	0.036 (3)	0.025 (3)
C5	0.072 (3)	0.128 (5)	0.063 (3)	0.038 (3)	0.000 (2)	0.032 (3)
C11	0.0309 (13)	0.0372 (14)	0.0237 (12)	−0.0014 (11)	0.0086 (10)	−0.0001 (10)
C12	0.082 (3)	0.054 (2)	0.0359 (17)	−0.0360 (19)	0.0250 (17)	−0.0119 (15)
C13	0.093 (3)	0.060 (2)	0.0412 (19)	−0.031 (2)	0.032 (2)	−0.0006 (17)
C14	0.057 (2)	0.0533 (19)	0.0266 (14)	−0.0024 (15)	0.0167 (13)	0.0005 (13)
C15	0.063 (2)	0.0421 (17)	0.0328 (16)	−0.0017 (15)	0.0193 (15)	−0.0071 (13)
C16	0.0542 (18)	0.0317 (14)	0.0340 (15)	−0.0021 (13)	0.0189 (13)	−0.0033 (12)
C21	0.0422 (16)	0.0473 (17)	0.0257 (13)	−0.0167 (13)	0.0092 (12)	0.0003 (12)
C22	0.0389 (16)	0.056 (2)	0.0420 (17)	−0.0096 (15)	0.0076 (13)	0.0092 (15)
C23	0.0400 (19)	0.093 (3)	0.058 (2)	−0.012 (2)	0.0076 (17)	0.027 (2)
C24	0.057 (3)	0.144 (5)	0.038 (2)	−0.049 (3)	−0.0010 (18)	0.013 (3)
C25	0.082 (3)	0.124 (4)	0.039 (2)	−0.062 (3)	0.014 (2)	−0.026 (2)
C26	0.069 (2)	0.075 (3)	0.0403 (18)	−0.034 (2)	0.0213 (17)	−0.0202 (18)
F1	0.085 (5)	0.086 (4)	0.118 (6)	−0.018 (4)	0.052 (4)	−0.042 (4)
F4	0.134 (9)	0.258 (16)	0.079 (6)	−0.013 (9)	−0.006 (5)	−0.046 (8)
F3	0.069 (4)	0.283 (12)	0.233 (10)	−0.071 (6)	0.077 (5)	−0.211 (10)
F2	0.198 (10)	0.049 (4)	0.219 (11)	0.002 (5)	0.016 (8)	0.000 (5)

Geometric parameters (Å, º)

Fe—S1	2.2770 (8)	C14—C15	1.370 (5)
Fe—S1^i	2.2770 (8)	C14—H14A	0.9400
Fe—P1^i	2.3060 (8)	C15—C16	1.395 (4)
Fe—P1	2.3060 (8)	C15—H15A	0.9400
Fe—S2	2.3078 (7)	C16—H16A	0.9400
Fe—S2^i	2.3078 (7)	C21—C26	1.389 (5)
P1—C21	1.823 (3)	C21—C22	1.396 (5)
P1—C11	1.826 (3)	C22—C23	1.398 (5)
P1—C1	1.834 (3)	C22—H22A	0.9400
S1—C2	1.723 (3)	C23—C24	1.387 (7)
S2—C2	1.709 (3)	C23—H23A	0.9400
N—C2	1.316 (4)	C24—C25	1.370 (8)
N—C5	1.457 (6)	C24—H24A	0.9400
N—C3	1.471 (6)	C25—C26	1.388 (6)
C1—C1^i	1.531 (6)	C25—H25A	0.9400
C1—H1A	0.9800	C26—H26A	0.9400
C1—H1B	0.9800	F1—F4^i	0.923 (12)
C3—H3A	0.9700	F1—B	1.348 (15)
C3—H3B	0.9700	F4—F1^i	0.923 (12)
C3—H3C	0.9700	F4—B^i	0.914 (17)
C5—H5A	0.9700	F4—B	1.382 (14)
C5—H5B	0.9700	F4—F4^i	1.45 (2)
C5—H5C	0.9700	F4—F2^i	1.486 (17)
C11—C16	1.387 (4)	F3—B	1.467 (14)
C11—C12	1.387 (4)	F2—B	1.388 (14)
C12—C13	1.386 (5)	F2—F4^i	1.486 (17)
C12—H12A	0.9400	B—F4^i	0.914 (17)
C13—C14	1.373 (5)	B—B^i	1.84 (3)
C13—H13A	0.9400
S1—Fe—S1^i	100.38 (4)	C12—C13—H13A	120.1
S1—Fe—P1^i	169.04 (3)	C15—C14—C13	120.1 (3)
S1^i—Fe—P1^i	87.77 (3)	C15—C14—H14A	120.0
S1—Fe—P1	87.77 (3)	C13—C14—H14A	120.0
S1^i—Fe—P1	169.04 (3)	C14—C15—C16	120.6 (3)
P1^i—Fe—P1	85.18 (4)	C14—C15—H15A	119.7
S1—Fe—S2	76.10 (3)	C16—C15—H15A	119.7
S1^i—Fe—S2	93.54 (3)	C11—C16—C15	119.9 (3)
P1^i—Fe—S2	96.23 (3)	C11—C16—H16A	120.1
P1—Fe—S2	95.56 (3)	C15—C16—H16A	120.1
S1—Fe—S2^i	93.54 (3)	C26—C21—C22	118.5 (3)
S1^i—Fe—S2^i	76.10 (3)	C26—C21—P1	122.3 (3)
P1^i—Fe—S2^i	95.56 (3)	C22—C21—P1	119.1 (2)
P1—Fe—S2^i	96.23 (3)	C21—C22—C23	121.1 (4)
S2—Fe—S2^i	163.97 (5)	C21—C22—H22A	119.4
C21—P1—C11	102.23 (13)	C23—C22—H22A	119.4
C21—P1—C1	105.84 (16)	C24—C23—C22	118.8 (5)
C11—P1—C1	102.53 (13)	C24—C23—H23A	120.6
C21—P1—Fe	115.57 (10)	C22—C23—H23A	120.6
C11—P1—Fe	120.84 (9)	C25—C24—C23	120.5 (4)
C1—P1—Fe	108.24 (10)	C25—C24—H24A	119.8
C2—S1—Fe	86.87 (11)	C23—C24—H24A	119.8
C2—S2—Fe	86.21 (11)	C24—C25—C26	120.7 (4)
C2—N—C5	120.8 (4)	C24—C25—H25A	119.7
C2—N—C3	120.5 (4)	C26—C25—H25A	119.7
C5—N—C3	118.6 (4)	C25—C26—C21	120.3 (5)
C1^i—C1—P1	110.48 (16)	C25—C26—H26A	119.8
C1^i—C1—H1A	109.6	C21—C26—H26A	119.8
P1—C1—H1A	109.6	F4^i—F1—B	42.5 (10)
C1^i—C1—H1B	109.6	F1^i—F4—B^i	94.4 (15)
P1—C1—H1B	109.6	F1^i—F4—B	130.5 (19)
H1A—C1—H1B	108.1	B^i—F4—B	104.6 (16)
N—C2—S2	125.4 (3)	F1^i—F4—F4^i	127.2 (12)
N—C2—S1	123.8 (3)	B^i—F4—F4^i	67.3 (15)
S2—C2—S1	110.82 (17)	B—F4—F4^i	37.6 (7)
N—C3—H3A	109.5	F1^i—F4—F2^i	125.5 (13)
N—C3—H3B	109.5	B^i—F4—F2^i	65.7 (14)
H3A—C3—H3B	109.5	B—F4—F2^i	103.9 (12)
N—C3—H3C	109.5	F4^i—F4—F2^i	92.6 (8)
H3A—C3—H3C	109.5	B—F2—F4^i	36.9 (7)
H3B—C3—H3C	109.5	F4^i—B—F2	77.4 (15)
N—C5—H5A	109.5	F4^i—B—F4	75.1 (16)
N—C5—H5B	109.5	F2—B—F4	100.0 (13)
H5A—C5—H5B	109.5	F4^i—B—F1	43.1 (10)
N—C5—H5C	109.5	F2—B—F1	104.1 (11)
H5A—C5—H5C	109.5	F4—B—F1	103.0 (13)
H5B—C5—H5C	109.5	F4^i—B—F3	149.0 (17)
C16—C11—C12	118.7 (3)	F2—B—F3	121.3 (13)
C16—C11—P1	123.3 (2)	F4—B—F3	120.1 (13)
C12—C11—P1	118.1 (2)	F1—B—F3	106.0 (10)
C13—C12—C11	121.1 (3)	F4^i—B—B^i	46.7 (11)
C13—C12—H12A	119.5	F2—B—B^i	87.7 (9)
C11—C12—H12A	119.5	F4—B—B^i	28.8 (8)
C14—C13—C12	119.7 (3)	F1—B—B^i	81.0 (11)
C14—C13—H13A	120.1	F3—B—B^i	145.8 (12)

Symmetry code: (i) −x+1, y, −z+1/2.