trans-Carbonyl­chloro­bis­[tris(2-methyl­phenyl)­phosphito]­rhodium(I)

The title compound, [Rh{P(OC₇H₇)₃}₂Cl(CO)], where P(OC₇H₇)₃ is tris(2-methyl­phenyl)­phosphite, crystallizes disordered over an inversion centre. Important geometrical parameters are Rh—P = 2.2905 (9) Å, Rh—Cl = 2.402 (4) Å, Rh—C = 1.764 (10) Å, and C—Rh—Cl = 177.7 (5)°, P—Rh—Cl = 85.84 (12)° and Rh—C[triple bond]O = 174.7 (15)°. The effective cone angle for the phosphite ligand was calculated to be 167°.

Key indicators

• Single-crystal X-ray study
• T = 292 K
• R factor = 0.040
• wR factor = 0.093
• Data-to-parameter ratio = 19.0

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT301_ALERT_3_C Main Residue  Disorder .........................       5.00 Perc.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   1 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
   1 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART-NT (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus and XPREP (Bruker, 1999); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Berndt, 2001); software used to prepare material for publication: WinGX (Farrugia, 1999).

(I)

Crystal data

[Rl(C21H21O3P)2Cl(CO)]	Z = 1
Mr = 871.07	F(000) = 448
Triclinic, P1	Dx = 1.379 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.1871 (16) Å	Cell parameters from 828 reflections
b = 10.785 (2) Å	θ = 2.7–24.3°
c = 13.101 (3) Å	µ = 0.59 mm^−1
α = 102.12 (3)°	T = 292 K
β = 104.65 (3)°	Plate, yellow
γ = 102.46 (3)°	0.48 × 0.22 × 0.11 mm
V = 1049.1 (5) Å^3

Data collection

Bruker SMART 1K CCD diffractometer	3453 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.019
ω scans	θmax = 28.3°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Bruker, 1998)	h = −10→10
Tmin = 0.764, Tmax = 0.938	k = −14→10
7011 measured reflections	l = −15→17
4966 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.040	w = 1/[σ^2(Fo^2) + (0.0405P)^2 + 0.1712P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.093	(Δ/σ)max = 0.001
S = 1.02	Δρmax = 0.30 e Å^−3
4966 reflections	Δρmin = −0.45 e Å^−3
262 parameters

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Rh	0.5	0	0.5	0.04413 (12)
P	0.56366 (9)	0.01962 (7)	0.68428 (5)	0.04387 (18)
Cl	0.6863 (5)	0.2167 (4)	0.5259 (4)	0.0599 (10)	0.5
O1	0.4111 (3)	0.01895 (18)	0.74017 (15)	0.0544 (5)
O2	0.7173 (2)	0.14983 (18)	0.75587 (14)	0.0501 (5)
O3	0.6140 (3)	−0.09935 (19)	0.72860 (15)	0.0563 (5)
C11	0.3198 (4)	0.1160 (3)	0.7463 (2)	0.0491 (7)
C21	0.7723 (4)	0.2050 (3)	0.8717 (2)	0.0510 (7)
C31	0.7065 (4)	−0.1809 (3)	0.6847 (2)	0.0508 (7)
C12	0.2988 (4)	0.1661 (3)	0.8469 (2)	0.0536 (7)
C16	0.2472 (4)	0.1533 (3)	0.6536 (2)	0.0639 (9)
H16	0.2617	0.1169	0.5867	0.077*
C36	0.8639 (4)	−0.1259 (3)	0.6699 (2)	0.0598 (8)
H36	0.9077	−0.0347	0.6855	0.072*
C32	0.6344 (5)	−0.3164 (3)	0.6643 (2)	0.0616 (9)
C22	0.7599 (4)	0.3295 (3)	0.9095 (2)	0.0632 (9)
C13	0.2038 (4)	0.2580 (3)	0.8522 (3)	0.0676 (9)
H13	0.1882	0.2942	0.9188	0.081*
C26	0.8472 (4)	0.1365 (3)	0.9400 (3)	0.0666 (9)
H26	0.8575	0.0531	0.9111	0.08*
C121	0.3753 (5)	0.1240 (4)	0.9472 (3)	0.0752 (10)
H12A	0.3554	0.0298	0.927	0.113*
H12B	0.3196	0.1484	1.0016	0.113*
H12C	0.4996	0.167	0.9769	0.113*
C35	0.9560 (5)	−0.2090 (4)	0.6313 (3)	0.0773 (10)
H35	1.0628	−0.1742	0.6209	0.093*
C15	0.1540 (5)	0.2444 (4)	0.6620 (3)	0.0759 (10)
H15	0.1056	0.2707	0.6007	0.091*
C33	0.7304 (7)	−0.3961 (4)	0.6244 (3)	0.0826 (12)
H33	0.6869	−0.4875	0.6081	0.099*
C221	0.6847 (5)	0.4057 (3)	0.8337 (3)	0.0793 (11)
H22A	0.7145	0.3845	0.7671	0.119*
H22B	0.733	0.4988	0.8693	0.119*
H22C	0.5589	0.3819	0.8168	0.119*
C34	0.8873 (7)	−0.3439 (5)	0.6085 (3)	0.0879 (13)
H34	0.9481	−0.4002	0.5821	0.105*
C14	0.1320 (5)	0.2970 (4)	0.7613 (3)	0.0795 (11)
H14	0.0687	0.3588	0.7671	0.095*
C23	0.8195 (6)	0.3845 (4)	1.0229 (3)	0.0983 (14)
H23	0.8103	0.4681	1.0522	0.118*
C25	0.9060 (5)	0.1949 (5)	1.0520 (3)	0.0883 (13)
H25	0.9553	0.1502	1.0994	0.106*
C24	0.8924 (7)	0.3169 (5)	1.0930 (3)	0.1085 (17)
H24	0.9322	0.3557	1.1685	0.13*
C321	0.4647 (6)	−0.3717 (4)	0.6845 (3)	0.0912 (12)
H32A	0.4352	−0.4665	0.6638	0.137*
H32B	0.3727	−0.3444	0.6416	0.137*
H32C	0.4778	−0.3396	0.7611	0.137*
C	0.6423 (19)	0.1587 (9)	0.5241 (11)	0.057 (3)	0.5
O	0.7346 (16)	0.2622 (10)	0.5480 (9)	0.062 (3)	0.5

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh	0.0519 (2)	0.0427 (2)	0.03684 (17)	0.01836 (16)	0.00901 (14)	0.00991 (13)
P	0.0478 (4)	0.0435 (4)	0.0404 (4)	0.0167 (4)	0.0107 (3)	0.0119 (3)
Cl	0.066 (3)	0.046 (3)	0.0448 (18)	0.000 (2)	−0.0034 (16)	0.006 (2)
O1	0.0576 (13)	0.0524 (12)	0.0571 (12)	0.0193 (10)	0.0210 (10)	0.0160 (9)
O2	0.0555 (12)	0.0522 (12)	0.0397 (10)	0.0101 (10)	0.0106 (9)	0.0174 (8)
O3	0.0753 (14)	0.0522 (12)	0.0529 (11)	0.0302 (11)	0.0226 (10)	0.0230 (9)
C11	0.0414 (16)	0.0520 (17)	0.0494 (16)	0.0101 (14)	0.0123 (13)	0.0102 (13)
C21	0.0472 (17)	0.0555 (18)	0.0377 (14)	0.0000 (14)	0.0033 (12)	0.0141 (13)
C31	0.064 (2)	0.0484 (17)	0.0385 (14)	0.0246 (16)	0.0055 (13)	0.0132 (12)
C12	0.0497 (18)	0.0581 (18)	0.0481 (16)	0.0066 (15)	0.0160 (13)	0.0125 (14)
C16	0.061 (2)	0.087 (2)	0.0446 (16)	0.0341 (19)	0.0130 (15)	0.0133 (16)
C36	0.063 (2)	0.061 (2)	0.0510 (17)	0.0215 (17)	0.0095 (15)	0.0133 (15)
C32	0.078 (2)	0.0496 (19)	0.0498 (17)	0.0195 (18)	0.0040 (16)	0.0174 (14)
C22	0.072 (2)	0.0488 (18)	0.0462 (17)	−0.0036 (16)	0.0011 (15)	0.0088 (14)
C13	0.070 (2)	0.081 (2)	0.0562 (19)	0.030 (2)	0.0260 (17)	0.0099 (17)
C26	0.060 (2)	0.071 (2)	0.0581 (19)	0.0096 (17)	0.0004 (16)	0.0287 (16)
C121	0.086 (3)	0.090 (3)	0.062 (2)	0.026 (2)	0.0320 (19)	0.0359 (19)
C35	0.076 (3)	0.105 (3)	0.058 (2)	0.044 (2)	0.0185 (18)	0.021 (2)
C15	0.074 (2)	0.104 (3)	0.060 (2)	0.048 (2)	0.0156 (18)	0.0263 (19)
C33	0.133 (4)	0.056 (2)	0.056 (2)	0.045 (2)	0.011 (2)	0.0158 (16)
C221	0.101 (3)	0.0444 (19)	0.075 (2)	0.0133 (19)	0.005 (2)	0.0147 (16)
C34	0.122 (4)	0.103 (3)	0.056 (2)	0.075 (3)	0.023 (2)	0.018 (2)
C14	0.079 (3)	0.092 (3)	0.077 (2)	0.049 (2)	0.025 (2)	0.019 (2)
C23	0.138 (4)	0.063 (2)	0.053 (2)	−0.002 (2)	0.002 (2)	−0.0023 (18)
C25	0.084 (3)	0.099 (3)	0.057 (2)	−0.001 (2)	−0.0115 (19)	0.038 (2)
C24	0.138 (4)	0.093 (3)	0.041 (2)	−0.018 (3)	−0.012 (2)	0.010 (2)
C321	0.106 (3)	0.065 (2)	0.093 (3)	0.009 (2)	0.014 (2)	0.036 (2)
C	0.073 (8)	0.039 (7)	0.042 (4)	0.016 (6)	0.001 (4)	−0.003 (5)
O	0.072 (7)	0.045 (6)	0.045 (5)	0.001 (4)	−0.003 (4)	0.008 (4)

Geometric parameters (Å, º)

Rh—C^i	1.764 (10)	C22—C221	1.513 (4)
Rh—C	1.764 (10)	C13—C14	1.380 (4)
Rh—P^i	2.2905 (9)	C13—H13	0.93
Rh—P	2.2905 (9)	C26—C25	1.380 (5)
Rh—Cl	2.402 (4)	C26—H26	0.93
Rh—Cl^i	2.402 (4)	C121—H12A	0.96
P—O2	1.588 (2)	C121—H12B	0.96
P—O1	1.599 (2)	C121—H12C	0.96
P—O3	1.6041 (19)	C35—C34	1.379 (6)
Cl—O	0.529 (8)	C35—H35	0.93
Cl—C	0.643 (8)	C15—C14	1.379 (5)
O1—C11	1.412 (3)	C15—H15	0.93
O2—C21	1.420 (3)	C33—C34	1.373 (6)
O3—C31	1.405 (3)	C33—H33	0.93
C11—C12	1.384 (4)	C221—H22A	0.96
C11—C16	1.391 (4)	C221—H22B	0.96
C21—C22	1.366 (4)	C221—H22C	0.96
C21—C26	1.385 (4)	C34—H34	0.93
C31—C36	1.376 (4)	C14—H14	0.93
C31—C32	1.393 (4)	C23—C24	1.386 (6)
C12—C13	1.386 (4)	C23—H23	0.93
C12—C121	1.511 (4)	C25—C24	1.352 (6)
C16—C15	1.371 (4)	C25—H25	0.93
C16—H16	0.93	C24—H24	0.93
C36—C35	1.386 (4)	C321—H32A	0.96
C36—H36	0.93	C321—H32B	0.96
C32—C33	1.393 (5)	C321—H32C	0.96
C32—C321	1.500 (5)	C—O	1.133 (14)
C22—C23	1.391 (4)
C^i—Rh—C	180.0 (4)	C14—C13—C12	121.7 (3)
C^i—Rh—P^i	92.1 (4)	C14—C13—H13	119.1
C—Rh—P^i	87.9 (4)	C12—C13—H13	119.1
C^i—Rh—P	87.9 (4)	C25—C26—C21	118.4 (3)
C—Rh—P	92.1 (4)	C25—C26—H26	120.8
P^i—Rh—P	180	C21—C26—H26	120.8
C^i—Rh—Cl	177.7 (5)	C12—C121—H12A	109.5
C—Rh—Cl	2.3 (5)	C12—C121—H12B	109.5
P^i—Rh—Cl	85.84 (12)	H12A—C121—H12B	109.5
P—Rh—Cl	94.16 (12)	C12—C121—H12C	109.5
C^i—Rh—Cl^i	2.3 (5)	H12A—C121—H12C	109.5
C—Rh—Cl^i	177.7 (5)	H12B—C121—H12C	109.5
P^i—Rh—Cl^i	94.16 (12)	C34—C35—C36	119.2 (4)
P—Rh—Cl^i	85.84 (12)	C34—C35—H35	120.4
Cl—Rh—Cl^i	180	C36—C35—H35	120.4
O2—P—O1	105.20 (11)	C16—C15—C14	119.9 (3)
O2—P—O3	106.33 (10)	C16—C15—H15	120
O1—P—O3	92.68 (11)	C14—C15—H15	120
O2—P—Rh	111.89 (8)	C34—C33—C32	122.0 (4)
O1—P—Rh	119.63 (8)	C34—C33—H33	119
O3—P—Rh	118.75 (8)	C32—C33—H33	119
O—Cl—C	150 (2)	C22—C221—H22A	109.5
O—Cl—Rh	157 (2)	C22—C221—H22B	109.5
C11—O1—P	124.20 (18)	H22A—C221—H22B	109.5
C21—O2—P	127.47 (18)	C22—C221—H22C	109.5
C31—O3—P	125.07 (18)	H22A—C221—H22C	109.5
C12—C11—C16	122.2 (3)	H22B—C221—H22C	109.5
C12—C11—O1	116.8 (3)	C33—C34—C35	120.8 (4)
C16—C11—O1	120.9 (3)	C33—C34—H34	119.6
C22—C21—C26	123.1 (3)	C35—C34—H34	119.6
C22—C21—O2	117.0 (2)	C15—C14—C13	120.0 (3)
C26—C21—O2	119.7 (3)	C15—C14—H14	120
C36—C31—C32	123.6 (3)	C13—C14—H14	120
C36—C31—O3	120.3 (3)	C24—C23—C22	121.2 (4)
C32—C31—O3	116.0 (3)	C24—C23—H23	119.4
C11—C12—C13	116.9 (3)	C22—C23—H23	119.4
C11—C12—C121	122.2 (3)	C24—C25—C26	120.3 (3)
C13—C12—C121	120.9 (3)	C24—C25—H25	119.8
C15—C16—C11	119.2 (3)	C26—C25—H25	119.8
C15—C16—H16	120.4	C25—C24—C23	120.3 (3)
C11—C16—H16	120.4	C25—C24—H24	119.9
C31—C36—C35	118.8 (3)	C23—C24—H24	119.9
C31—C36—H36	120.6	C32—C321—H32A	109.5
C35—C36—H36	120.6	C32—C321—H32B	109.5
C31—C32—C33	115.5 (3)	H32A—C321—H32B	109.5
C31—C32—C321	121.8 (3)	C32—C321—H32C	109.5
C33—C32—C321	122.6 (3)	H32A—C321—H32C	109.5
C21—C22—C23	116.6 (3)	H32B—C321—H32C	109.5
C21—C22—C221	122.7 (3)	Cl—C—Rh	171.2 (18)
C23—C22—C221	120.7 (3)	O—C—Rh	174.7 (15)
C—Rh—P—O1	116.7 (5)	C—Rh—P—O3	−131.4 (5)
C—Rh—P—O2	−6.9 (5)

Symmetry code: (i) −x+1, −y, −z+1.