(η⁴-Norbornadiene)bis­(tetra­hydro­furan-κO)rhodium(I) tetra­fluoro­borate

The title complex, [Rh(C₇H₈)(C₄H₈O)₂]BF₄, contains a rhodium(I) centre coordinated in a square-planar manner by two tetra­hydro­furan mol­ecules and the mid-points of the double bonds of an η⁴-coordinated norbornadiene ligand.

Key indicators

• Single-crystal X-ray study
• T = 110 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.032
• wR factor = 0.090
• Data-to-parameter ratio = 20.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT028_ALERT_3_C _diffrn_measured_fraction_theta_max  Low .......       0.94
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.95
PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size .......       0.70 mm
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 =          3
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for         B1

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   6 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
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 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

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Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97.

(η⁴-Norbornadiene)bis(tetrahydrofuran-κO)rhodium(I) tetrafluoroborate

Crystal data

[Rh(C7H8)(C4H8O)2]BF4	F(000) = 864
Mr = 426.06	Dx = 1.682 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 12.010 (6) Å	Cell parameters from 8096 reflections
b = 9.580 (5) Å	θ = 2.4–28.5°
c = 17.098 (7) Å	µ = 1.06 mm^−1
β = 121.20 (3)°	T = 110 K
V = 1682.7 (14) Å^3	Plate, yellow
Z = 4	0.70 × 0.52 × 0.48 mm

Data collection

Bruker SMART APEX CCD diffractometer	4213 independent reflections
Radiation source: fine-focus sealed tube	3563 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.056
ω scans	θmax = 28.5°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −16→16
Tmin = 0.524, Tmax = 0.630	k = −12→12
20904 measured reflections	l = −22→22

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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.090	H-atom parameters constrained
S = 1.00	w = 1/[σ^2(Fo^2) + (0.075P)^2] where P = (Fo^2 + 2Fc^2)/3
4213 reflections	(Δ/σ)max = 0.001
208 parameters	Δρmax = 1.35 e Å^−3
0 restraints	Δρmin = −0.75 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
Rh1	0.260984 (18)	0.71140 (2)	0.049538 (13)	0.01940 (8)
O1	0.35728 (18)	0.51709 (19)	0.11062 (13)	0.0254 (4)
O2	0.1553 (2)	0.6858 (2)	0.11960 (16)	0.0313 (4)
C1	0.4023 (3)	0.4218 (3)	0.06574 (19)	0.0282 (6)
H1A	0.4674	0.4665	0.0558	0.037*
H1B	0.3297	0.3891	0.0070	0.037*
C2	0.4620 (3)	0.3023 (3)	0.1346 (2)	0.0290 (6)
H2A	0.5208	0.2447	0.1233	0.038*
H2B	0.3940	0.2419	0.1330	0.038*
C3	0.5379 (3)	0.3820 (3)	0.2257 (2)	0.0318 (6)
H3A	0.5444	0.3261	0.2766	0.041*
H3B	0.6267	0.4056	0.2398	0.041*
C4	0.4571 (3)	0.5139 (3)	0.2097 (2)	0.0326 (6)
H4A	0.4155	0.5112	0.2461	0.042*
H4B	0.5125	0.5970	0.2270	0.042*
C5	0.0653 (3)	0.7896 (3)	0.1182 (2)	0.0327 (6)
H5A	0.0594	0.8708	0.0814	0.042*
H5B	0.0930	0.8208	0.1803	0.042*
C6	−0.0641 (3)	0.7135 (3)	0.0755 (3)	0.0385 (7)
H6A	−0.1082	0.7122	0.0080	0.050*
H6B	−0.1226	0.7567	0.0934	0.050*
C7	−0.0226 (3)	0.5648 (3)	0.1159 (2)	0.0336 (6)
H7A	−0.0246	0.5555	0.1729	0.044*
H7B	−0.0809	0.4936	0.0716	0.044*
C8	0.1154 (3)	0.5485 (3)	0.1353 (2)	0.0307 (6)
H8A	0.1739	0.5187	0.1987	0.040*
H8B	0.1180	0.4786	0.0945	0.040*
C9	0.2907 (3)	0.7165 (3)	−0.06120 (19)	0.0234 (5)
H9	0.3038	0.6323	−0.0880	0.030*
C10	0.3939 (3)	0.7878 (3)	0.01435 (19)	0.0247 (5)
H10	0.4851	0.7580	0.0447	0.032*
C11	0.3514 (3)	0.9427 (3)	0.0031 (2)	0.0284 (6)
H11	0.4191	1.0123	0.0383	0.037*
C12	0.2397 (3)	0.9282 (3)	0.0237 (2)	0.0267 (5)
H12	0.2257	0.9950	0.0612	0.035*
C13	0.1375 (3)	0.8580 (3)	−0.05196 (18)	0.0253 (5)
H13	0.0552	0.8338	−0.0604	0.033*
C14	0.1857 (3)	0.8281 (3)	−0.11847 (19)	0.0277 (5)
H14	0.1201	0.8041	−0.1817	0.036*
C15	0.2722 (3)	0.9586 (3)	−0.1029 (2)	0.0345 (6)
H15A	0.2215	1.0465	−0.1235	0.045*
H15B	0.3267	0.9488	−0.1305	0.045*
F1	0.2005 (2)	0.1284 (3)	0.17471 (15)	0.0578 (6)
F2	0.2706 (3)	0.0930 (3)	0.3267 (2)	0.0844 (10)
F3	0.12034 (17)	0.2632 (2)	0.24560 (14)	0.0387 (4)
F4	0.3306 (2)	0.2842 (2)	0.28153 (18)	0.0558 (6)
B1	0.2272 (3)	0.1880 (4)	0.2566 (2)	0.0291 (6)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.01836 (11)	0.01895 (12)	0.02000 (12)	0.00196 (7)	0.00930 (9)	0.00205 (7)
O1	0.0275 (9)	0.0249 (9)	0.0240 (9)	0.0051 (7)	0.0135 (8)	0.0027 (7)
O2	0.0346 (11)	0.0239 (9)	0.0444 (12)	0.0036 (8)	0.0269 (10)	0.0054 (9)
C1	0.0302 (13)	0.0272 (13)	0.0301 (14)	0.0068 (11)	0.0177 (12)	0.0022 (11)
C2	0.0329 (14)	0.0238 (13)	0.0342 (15)	0.0068 (10)	0.0201 (13)	0.0038 (11)
C3	0.0245 (13)	0.0282 (14)	0.0325 (15)	0.0006 (11)	0.0074 (11)	0.0053 (12)
C4	0.0342 (15)	0.0292 (14)	0.0267 (14)	0.0040 (12)	0.0103 (12)	−0.0006 (12)
C5	0.0405 (16)	0.0261 (14)	0.0453 (18)	0.0027 (11)	0.0321 (15)	−0.0010 (12)
C6	0.0329 (16)	0.0373 (17)	0.050 (2)	0.0042 (12)	0.0244 (15)	−0.0038 (14)
C7	0.0312 (14)	0.0338 (15)	0.0396 (16)	−0.0074 (12)	0.0209 (13)	−0.0072 (13)
C8	0.0329 (14)	0.0264 (13)	0.0378 (16)	0.0009 (11)	0.0219 (13)	0.0074 (12)
C9	0.0241 (12)	0.0241 (13)	0.0234 (13)	0.0027 (10)	0.0134 (11)	0.0012 (10)
C10	0.0220 (12)	0.0279 (13)	0.0260 (13)	0.0013 (10)	0.0136 (11)	0.0033 (10)
C11	0.0303 (13)	0.0248 (13)	0.0335 (15)	−0.0047 (11)	0.0188 (12)	−0.0020 (11)
C12	0.0313 (13)	0.0221 (13)	0.0308 (14)	0.0020 (10)	0.0190 (12)	0.0007 (11)
C13	0.0241 (12)	0.0263 (13)	0.0246 (12)	0.0067 (10)	0.0118 (10)	0.0069 (11)
C14	0.0263 (13)	0.0346 (14)	0.0192 (12)	0.0072 (11)	0.0097 (11)	0.0045 (11)
C15	0.0443 (17)	0.0308 (15)	0.0392 (16)	0.0092 (12)	0.0292 (15)	0.0112 (13)
F1	0.0432 (11)	0.0752 (16)	0.0472 (12)	0.0065 (11)	0.0179 (10)	−0.0263 (11)
F2	0.110 (2)	0.0799 (19)	0.100 (2)	0.0497 (17)	0.080 (2)	0.0553 (17)
F3	0.0257 (9)	0.0421 (10)	0.0466 (11)	0.0020 (8)	0.0175 (8)	−0.0084 (9)
F4	0.0338 (11)	0.0604 (15)	0.0704 (16)	−0.0102 (9)	0.0250 (11)	−0.0142 (11)
B1	0.0264 (15)	0.0319 (16)	0.0294 (16)	0.0044 (12)	0.0147 (13)	0.0010 (13)

Geometric parameters (Å, º)

Rh1—C9	2.101 (3)	C6—H6B	0.9900
Rh1—C10	2.108 (3)	C7—C8	1.520 (4)
Rh1—C12	2.112 (3)	C7—H7A	0.9900
Rh1—C13	2.125 (3)	C7—H7B	0.9900
Rh1—O1	2.155 (2)	C8—H8A	0.9800
Rh1—O2	2.163 (2)	C8—H8B	0.9800
O1—C1	1.464 (3)	C9—C10	1.419 (4)
O1—C4	1.484 (3)	C9—C14	1.553 (4)
O2—C5	1.460 (3)	C9—H9	0.9800
O2—C8	1.471 (3)	C10—C11	1.549 (4)
C1—C2	1.529 (4)	C10—H10	0.9800
C1—H1A	0.9800	C11—C15	1.559 (4)
C1—H1B	0.9800	C11—C12	1.559 (4)
C2—C3	1.539 (4)	C11—H11	0.9800
C2—H2A	0.9900	C12—C13	1.410 (4)
C2—H2B	0.9900	C12—H12	0.9800
C3—C4	1.529 (4)	C13—C14	1.547 (4)
C3—H3A	0.9900	C13—H13	0.9500
C3—H3B	0.9900	C14—C15	1.558 (4)
C4—H4A	0.9800	C14—H14	0.9800
C4—H4B	0.9800	C15—H15A	0.9900
C5—C6	1.518 (4)	C15—H15B	0.9900
C5—H5A	0.9800	F1—B1	1.386 (4)
C5—H5B	0.9800	F2—B1	1.374 (4)
C6—C7	1.548 (4)	F3—B1	1.397 (4)
C6—H6A	0.9900	F4—B1	1.422 (4)
C9—Rh1—C10	39.40 (11)	C6—C7—H7A	110.8
C9—Rh1—C12	81.20 (10)	C8—C7—H7B	110.8
C10—Rh1—C12	68.04 (10)	C6—C7—H7B	110.8
C9—Rh1—C13	67.73 (10)	H7A—C7—H7B	108.9
C10—Rh1—C13	81.31 (11)	O2—C8—C7	106.9 (2)
C12—Rh1—C13	38.87 (11)	O2—C8—H8A	110.4
C9—Rh1—O1	99.09 (9)	C7—C8—H8A	110.4
C10—Rh1—O1	98.20 (9)	O2—C8—H8B	110.4
C12—Rh1—O1	158.09 (9)	C7—C8—H8B	110.4
C13—Rh1—O1	159.89 (9)	H8A—C8—H8B	108.6
C9—Rh1—O2	157.48 (10)	C10—C9—C14	106.5 (2)
C10—Rh1—O2	161.05 (10)	C10—C9—Rh1	70.56 (16)
C12—Rh1—O2	100.69 (9)	C14—C9—Rh1	97.07 (16)
C13—Rh1—O2	99.54 (9)	C10—C9—H9	123.1
O1—Rh1—O2	87.43 (8)	C14—C9—H9	123.1
C1—O1—C4	106.6 (2)	Rh1—C9—H9	123.1
C1—O1—Rh1	122.39 (15)	C9—C10—C11	105.8 (2)
C4—O1—Rh1	118.98 (16)	C9—C10—Rh1	70.04 (15)
C5—O2—C8	107.6 (2)	C11—C10—Rh1	96.77 (16)
C5—O2—Rh1	123.79 (17)	C9—C10—H10	123.5
C8—O2—Rh1	122.86 (16)	C11—C10—H10	123.5
O1—C1—C2	102.5 (2)	Rh1—C10—H10	123.5
O1—C1—H1A	111.3	C10—C11—C15	101.6 (2)
C2—C1—H1A	111.3	C10—C11—C12	98.8 (2)
O1—C1—H1B	111.3	C15—C11—C12	101.1 (2)
C2—C1—H1B	111.3	C10—C11—H11	117.4
H1A—C1—H1B	109.2	C15—C11—H11	117.4
C1—C2—C3	101.7 (2)	C12—C11—H11	117.4
C1—C2—H2A	111.4	C13—C12—C11	106.1 (2)
C3—C2—H2A	111.4	C13—C12—Rh1	71.09 (16)
C1—C2—H2B	111.4	C11—C12—Rh1	96.32 (16)
C3—C2—H2B	111.4	C13—C12—H12	123.3
H2A—C2—H2B	109.3	C11—C12—H12	123.3
C4—C3—C2	103.9 (2)	Rh1—C12—H12	123.3
C4—C3—H3A	111.0	C12—C13—C14	106.5 (2)
C2—C3—H3A	111.0	C12—C13—Rh1	70.04 (16)
C4—C3—H3B	111.0	C14—C13—Rh1	96.27 (16)
C2—C3—H3B	111.0	C12—C13—H13	126.8
H3A—C3—H3B	109.0	C14—C13—H13	126.8
O1—C4—C3	106.5 (2)	Rh1—C13—H13	101.2
O1—C4—H4A	110.4	C13—C14—C9	98.9 (2)
C3—C4—H4A	110.4	C13—C14—C15	101.3 (2)
O1—C4—H4B	110.4	C9—C14—C15	101.2 (2)
C3—C4—H4B	110.4	C13—C14—H14	117.4
H4A—C4—H4B	108.6	C9—C14—H14	117.4
O2—C5—C6	104.2 (2)	C15—C14—H14	117.4
O2—C5—H5A	110.9	C14—C15—C11	94.1 (2)
C6—C5—H5A	110.9	C14—C15—H15A	112.9
O2—C5—H5B	110.9	C11—C15—H15A	112.9
C6—C5—H5B	110.9	C14—C15—H15B	112.9
H5A—C5—H5B	108.9	C11—C15—H15B	112.9
C5—C6—C7	102.4 (3)	H15A—C15—H15B	110.3
C5—C6—H6A	111.3	F2—B1—F1	113.1 (3)
C7—C6—H6A	111.3	F2—B1—F3	111.4 (3)
C5—C6—H6B	111.3	F1—B1—F3	111.1 (3)
C7—C6—H6B	111.3	F2—B1—F4	106.8 (3)
H6A—C6—H6B	109.2	F1—B1—F4	106.2 (3)
C8—C7—C6	104.8 (2)	F3—B1—F4	107.7 (3)
C8—C7—H7A	110.8