{2,6-Bis­[(di­phenyl­phosphino)­methyl]­phenyl}chloro­platinum(II)

The title compound, [PtCl(C₃₂H₂₇P₂)], has a pseudo-square-planar coordination geometry around the Pt atom with the P,C,P'-tridentate ligand forming two five-membered rings that are tilted with respect to the coordination plane. The two Pt-P, the Pt-Cl and the Pt-C distances are 2.2794 (9)/2.2749 (10), 2.3831 (10) and 2.002 (3) Å, respectively.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.027
• wR factor = 0.041
• Data-to-parameter ratio = 26.2

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.91

Alert level C
REFLT03_ALERT_3_C  Reflection count < 95% complete
           From the CIF: _diffrn_reflns_theta_max           31.81
           From the CIF: _diffrn_reflns_theta_full           0.00
           From the CIF: _reflns_number_total               8500
           TEST2: Reflns within _diffrn_reflns_theta_max
           Count of symmetry unique reflns         9384
           Completeness (_total/calc)             90.58%
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       2.71 Ratio
PLAT230_ALERT_2_C Hirshfeld Test Diff for    C44    -   C45      =       6.18 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Pt1    -   C1       =       5.19 su
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....        C33
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....        C31
PLAT331_ALERT_2_C Small Av. Phenyl C-C Dist. C41    -   C46      =       1.37 Ang.

   1 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   8 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
   2 ALERT type 3 Indicator that the structure quality may be low
   1 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; molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.

{2,6-Bis[(diphenylphosphino)methyl]phenyl}chloroplatinum(II)

Crystal data

[PtCl(C32H27P2)]	F(000) = 1376
Mr = 704.02	Dx = 1.704 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 10.290 (2) Å	Cell parameters from 6134 reflections
b = 16.117 (3) Å	θ = 2.4–24.8°
c = 17.173 (3) Å	µ = 5.35 mm^−1
β = 105.47 (3)°	T = 293 K
V = 2744.8 (10) Å^3	Prism, yellow
Z = 4	0.25 × 0.20 × 0.12 mm

Data collection

Siemens SMART CCD diffractometer	8500 independent reflections
Radiation source: rotating anode	4739 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.049
Detector resolution: 512 pixels mm^-1	θmax = 31.8°, θmin = 1.8°
ω scans	h = −14→13
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −22→22
Tmin = 0.312, Tmax = 0.526	l = −25→25
27382 measured reflections

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)] = 0.027	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.041	H-atom parameters constrained
S = 0.91	w = 1/[σ^2(Fo^2) + (0.0001P)^2] where P = (Fo^2 + 2Fc^2)/3
8500 reflections	(Δ/σ)max = 0.004
325 parameters	Δρmax = 0.77 e Å^−3
0 restraints	Δρmin = −1.10 e Å^−3

Special details

Experimental. Data was collected with a SMART CCD system using ω-scan, -0.2° and 10 s per frame. The detector distance was set to 4.0 cm. The data have a completeness of more then 99% out to θ=29.3°. The structure was solved by direct methods and refined by full matrix least squares methods.

Scattering factors, dispersion corrections and absorption coefficients were taken from International Tables for Crystallography, Vol. C. (1992), tables 6.1.1.4, 4.2.6.8 and 4.2.4.2 respectively.

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
Pt1	0.996496 (13)	0.202660 (8)	0.969368 (8)	0.03471 (4)
P2	0.94856 (9)	0.24827 (6)	1.08397 (5)	0.0381 (2)
P1	1.09047 (9)	0.13474 (5)	0.88138 (5)	0.0378 (2)
Cl1	0.84548 (8)	0.29183 (6)	0.87706 (5)	0.0543 (2)
C1	1.1193 (3)	0.12616 (18)	1.04738 (18)	0.0352 (8)
C2	1.1704 (3)	0.05328 (19)	1.02204 (18)	0.0368 (8)
C3	1.2464 (4)	−0.0025 (2)	1.0770 (2)	0.0519 (10)
H3	1.2761	−0.0516	1.0589	0.062*
C4	1.2780 (4)	0.0147 (2)	1.1588 (2)	0.0554 (11)
H4	1.3300	−0.0227	1.1955	0.066*
C5	1.2335 (3)	0.0861 (2)	1.1864 (2)	0.0486 (9)
H5	1.2557	0.0973	1.2415	0.058*
C6	1.1555 (3)	0.1415 (2)	1.1322 (2)	0.0399 (8)
C7	1.1343 (3)	0.03528 (19)	0.93244 (18)	0.0422 (9)
H7A	1.0585	−0.0026	0.9177	0.051*
H7B	1.2102	0.0105	0.9176	0.051*
C8	1.1034 (3)	0.22054 (19)	1.16107 (18)	0.0465 (9)
H8A	1.1697	0.2645	1.1671	0.056*
H8B	1.0844	0.2116	1.2128	0.056*
C11	1.0091 (3)	0.1156 (2)	0.77538 (19)	0.0432 (9)
C12	0.9816 (4)	0.0367 (2)	0.7431 (2)	0.0655 (12)
H12	1.0037	−0.0094	0.7767	0.079*
C13	0.9217 (4)	0.0256 (3)	0.6614 (2)	0.0764 (13)
H13	0.9024	−0.0277	0.6408	0.092*
C14	0.8910 (4)	0.0921 (3)	0.6110 (2)	0.0746 (13)
H14	0.8514	0.0843	0.5561	0.090*
C15	0.9185 (4)	0.1704 (3)	0.6412 (2)	0.0709 (13)
H15	0.8994	0.2159	0.6068	0.085*
C16	0.9749 (4)	0.1821 (2)	0.7231 (2)	0.0577 (11)
H16	0.9900	0.2357	0.7434	0.069*
C21	1.2506 (3)	0.1803 (2)	0.87760 (19)	0.0392 (9)
C22	1.2910 (4)	0.2563 (2)	0.9154 (2)	0.0502 (10)
H22	1.2363	0.2835	0.9424	0.060*
C23	1.4125 (4)	0.2910 (3)	0.9126 (2)	0.0686 (11)
H23	1.4395	0.3413	0.9384	0.082*
C24	1.4937 (4)	0.2523 (3)	0.8723 (2)	0.0691 (13)
H24	1.5744	0.2768	0.8700	0.083*
C25	1.4565 (4)	0.1784 (3)	0.8358 (2)	0.0718 (14)
H25	1.5127	0.1523	0.8090	0.086*
C26	1.3353 (4)	0.1409 (2)	0.8376 (2)	0.0569 (11)
H26	1.3110	0.0900	0.8124	0.068*
C31	0.9186 (4)	0.3577 (2)	1.09825 (19)	0.0452 (9)
C32	0.8006 (4)	0.3873 (3)	1.1112 (2)	0.0725 (13)
H32	0.7316	0.3512	1.1143	0.087*
C33	0.7873 (5)	0.4717 (3)	1.1196 (3)	0.0958 (17)
H33	0.7065	0.4922	1.1262	0.115*
C34	0.8884 (5)	0.5262 (3)	1.1185 (2)	0.0773 (14)
H34	0.8785	0.5825	1.1276	0.093*
C35	1.0028 (5)	0.4973 (2)	1.1042 (3)	0.0775 (14)
H35	1.0707	0.5340	1.1006	0.093*
C36	1.0193 (4)	0.4126 (2)	1.0948 (2)	0.0741 (13)
H36	1.0992	0.3928	1.0860	0.089*
C41	0.8107 (3)	0.19309 (19)	1.10800 (19)	0.0381 (8)
C42	0.8153 (4)	0.1666 (2)	1.1852 (2)	0.0649 (12)
H42	0.8919	0.1754	1.2276	0.078*
C43	0.7032 (5)	0.1263 (3)	1.1985 (3)	0.0846 (15)
H43	0.7060	0.1082	1.2503	0.102*
C44	0.5905 (4)	0.1129 (3)	1.1380 (3)	0.0789 (14)
H44	0.5165	0.0863	1.1481	0.095*
C45	0.5870 (4)	0.1389 (2)	1.0625 (3)	0.0648 (12)
H45	0.5102	0.1300	1.0203	0.078*
C46	0.6954 (4)	0.1779 (2)	1.0481 (2)	0.0536 (10)
H46	0.6911	0.1949	0.9957	0.064*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pt1	0.03778 (8)	0.03177 (7)	0.03718 (7)	−0.00009 (8)	0.01454 (5)	−0.00031 (7)
P2	0.0431 (6)	0.0339 (5)	0.0389 (5)	0.0034 (4)	0.0137 (4)	−0.0029 (4)
P1	0.0425 (6)	0.0351 (5)	0.0396 (5)	0.0003 (4)	0.0177 (4)	−0.0014 (4)
Cl1	0.0525 (6)	0.0542 (6)	0.0552 (5)	0.0119 (5)	0.0125 (4)	0.0155 (5)
C1	0.036 (2)	0.0293 (18)	0.046 (2)	−0.0030 (16)	0.0197 (16)	−0.0075 (15)
C2	0.041 (2)	0.0335 (19)	0.040 (2)	0.0015 (17)	0.0178 (17)	0.0045 (16)
C3	0.066 (3)	0.041 (2)	0.054 (2)	0.0122 (19)	0.024 (2)	0.0066 (18)
C4	0.067 (3)	0.049 (2)	0.048 (2)	0.018 (2)	0.013 (2)	0.0182 (19)
C5	0.055 (3)	0.049 (2)	0.039 (2)	0.008 (2)	0.0090 (18)	0.0031 (18)
C6	0.033 (2)	0.039 (2)	0.047 (2)	−0.0006 (17)	0.0109 (17)	−0.0056 (17)
C7	0.045 (2)	0.033 (2)	0.051 (2)	0.0008 (16)	0.0168 (18)	0.0002 (16)
C8	0.049 (2)	0.045 (2)	0.043 (2)	0.0030 (18)	0.0075 (17)	−0.0077 (16)
C11	0.042 (2)	0.049 (2)	0.042 (2)	−0.0097 (18)	0.0188 (17)	−0.0055 (18)
C12	0.088 (3)	0.057 (3)	0.054 (3)	−0.010 (2)	0.023 (2)	−0.006 (2)
C13	0.097 (4)	0.081 (3)	0.050 (3)	−0.018 (3)	0.019 (3)	−0.027 (3)
C14	0.059 (3)	0.119 (4)	0.043 (3)	−0.005 (3)	0.007 (2)	−0.008 (3)
C15	0.070 (3)	0.090 (4)	0.047 (3)	−0.001 (3)	0.006 (2)	0.008 (2)
C16	0.065 (3)	0.053 (3)	0.053 (3)	−0.001 (2)	0.012 (2)	0.002 (2)
C21	0.036 (2)	0.047 (2)	0.035 (2)	0.0026 (17)	0.0098 (16)	0.0072 (16)
C22	0.049 (3)	0.055 (2)	0.049 (2)	−0.010 (2)	0.0176 (19)	0.0037 (18)
C23	0.059 (3)	0.080 (3)	0.061 (3)	−0.020 (3)	0.006 (2)	0.009 (2)
C24	0.042 (3)	0.099 (4)	0.063 (3)	−0.007 (3)	0.009 (2)	0.030 (3)
C25	0.059 (3)	0.099 (4)	0.072 (3)	0.023 (3)	0.042 (3)	0.033 (3)
C26	0.059 (3)	0.062 (3)	0.057 (3)	0.009 (2)	0.027 (2)	0.006 (2)
C31	0.062 (3)	0.037 (2)	0.040 (2)	0.0001 (19)	0.0190 (19)	−0.0021 (16)
C32	0.068 (3)	0.051 (3)	0.117 (4)	0.012 (2)	0.057 (3)	0.005 (3)
C33	0.115 (4)	0.059 (3)	0.142 (5)	0.023 (3)	0.084 (4)	−0.002 (3)
C34	0.124 (5)	0.044 (3)	0.075 (3)	0.013 (3)	0.046 (3)	−0.005 (2)
C35	0.102 (4)	0.039 (3)	0.100 (4)	−0.014 (3)	0.043 (3)	−0.005 (2)
C36	0.074 (3)	0.046 (3)	0.113 (4)	−0.010 (2)	0.043 (3)	−0.014 (2)
C41	0.050 (2)	0.0289 (19)	0.038 (2)	0.0006 (18)	0.0175 (17)	−0.0025 (16)
C42	0.089 (4)	0.064 (3)	0.046 (3)	−0.025 (2)	0.025 (2)	−0.011 (2)
C43	0.127 (5)	0.081 (3)	0.061 (3)	−0.027 (3)	0.050 (3)	0.005 (3)
C44	0.076 (4)	0.068 (3)	0.108 (4)	−0.022 (3)	0.050 (3)	−0.012 (3)
C45	0.044 (3)	0.076 (3)	0.075 (3)	−0.007 (2)	0.016 (2)	0.011 (2)
C46	0.047 (3)	0.058 (3)	0.058 (3)	0.004 (2)	0.019 (2)	0.0084 (19)

Geometric parameters (Å, º)

Pt1—C1	2.002 (3)	C16—H16	0.9300
Pt1—P2	2.2749 (10)	C21—C22	1.397 (4)
Pt1—P1	2.2794 (9)	C21—C26	1.398 (4)
Pt1—Cl1	2.3831 (10)	C22—C23	1.382 (4)
P2—C41	1.812 (3)	C22—H22	0.9300
P2—C31	1.819 (3)	C23—C24	1.368 (5)
P2—C8	1.835 (3)	C23—H23	0.9300
P1—C11	1.816 (3)	C24—C25	1.352 (5)
P1—C21	1.821 (3)	C24—H24	0.9300
P1—C7	1.825 (3)	C25—C26	1.394 (5)
C1—C2	1.403 (4)	C25—H25	0.9300
C1—C6	1.426 (4)	C26—H26	0.9300
C2—C3	1.385 (4)	C31—C36	1.375 (4)
C2—C7	1.511 (4)	C31—C32	1.377 (4)
C3—C4	1.384 (4)	C32—C33	1.378 (5)
C3—H3	0.9300	C32—H32	0.9300
C4—C5	1.370 (4)	C33—C34	1.366 (5)
C4—H4	0.9300	C33—H33	0.9300
C5—C6	1.381 (4)	C34—C35	1.349 (5)
C5—H5	0.9300	C34—H34	0.9300
C6—C8	1.515 (4)	C35—C36	1.391 (5)
C7—H7A	0.9700	C35—H35	0.9300
C7—H7B	0.9700	C36—H36	0.9300
C8—H8A	0.9700	C41—C46	1.369 (4)
C8—H8B	0.9700	C41—C42	1.381 (4)
C11—C16	1.382 (4)	C42—C43	1.395 (5)
C11—C12	1.385 (5)	C42—H42	0.9300
C12—C13	1.385 (5)	C43—C44	1.352 (5)
C12—H12	0.9300	C43—H43	0.9300
C13—C14	1.361 (5)	C44—C45	1.353 (5)
C13—H13	0.9300	C44—H44	0.9300
C14—C15	1.364 (5)	C45—C46	1.359 (4)
C14—H14	0.9300	C45—H45	0.9300
C15—C16	1.384 (5)	C46—H46	0.9300
C15—H15	0.9300
C1—Pt1—P2	82.18 (9)	C14—C15—C16	120.0 (4)
C1—Pt1—P1	81.04 (9)	C14—C15—H15	120.0
P2—Pt1—P1	163.11 (3)	C16—C15—H15	120.0
C1—Pt1—Cl1	178.53 (9)	C11—C16—C15	121.3 (4)
P2—Pt1—Cl1	97.31 (4)	C11—C16—H16	119.3
P1—Pt1—Cl1	99.51 (3)	C15—C16—H16	119.3
C41—P2—C31	105.93 (16)	C22—C21—C26	118.6 (3)
C41—P2—C8	107.33 (16)	C22—C21—P1	119.8 (3)
C31—P2—C8	106.54 (15)	C26—C21—P1	121.6 (3)
C41—P2—Pt1	113.69 (11)	C23—C22—C21	119.9 (4)
C31—P2—Pt1	120.91 (11)	C23—C22—H22	120.0
C8—P2—Pt1	101.46 (11)	C21—C22—H22	120.0
C11—P1—C21	102.28 (15)	C24—C23—C22	120.9 (4)
C11—P1—C7	108.71 (16)	C24—C23—H23	119.6
C21—P1—C7	105.15 (15)	C22—C23—H23	119.6
C11—P1—Pt1	125.62 (11)	C25—C24—C23	120.0 (4)
C21—P1—Pt1	112.21 (11)	C25—C24—H24	120.0
C7—P1—Pt1	101.39 (10)	C23—C24—H24	120.0
C2—C1—C6	116.4 (3)	C24—C25—C26	121.0 (4)
C2—C1—Pt1	122.0 (2)	C24—C25—H25	119.5
C6—C1—Pt1	121.5 (2)	C26—C25—H25	119.5
C3—C2—C1	121.5 (3)	C25—C26—C21	119.5 (4)
C3—C2—C7	120.7 (3)	C25—C26—H26	120.2
C1—C2—C7	117.8 (3)	C21—C26—H26	120.2
C4—C3—C2	119.9 (3)	C36—C31—C32	119.5 (3)
C4—C3—H3	120.0	C36—C31—P2	117.4 (3)
C2—C3—H3	120.0	C32—C31—P2	123.1 (3)
C5—C4—C3	120.7 (3)	C31—C32—C33	118.3 (4)
C5—C4—H4	119.7	C31—C32—H32	120.8
C3—C4—H4	119.7	C33—C32—H32	120.8
C4—C5—C6	119.9 (3)	C34—C33—C32	122.5 (4)
C4—C5—H5	120.0	C34—C33—H33	118.8
C6—C5—H5	120.0	C32—C33—H33	118.8
C5—C6—C1	121.5 (3)	C35—C34—C33	119.0 (4)
C5—C6—C8	121.1 (3)	C35—C34—H34	120.5
C1—C6—C8	117.4 (3)	C33—C34—H34	120.5
C2—C7—P1	106.4 (2)	C34—C35—C36	120.1 (4)
C2—C7—H7A	110.4	C34—C35—H35	120.0
P1—C7—H7A	110.4	C36—C35—H35	120.0
C2—C7—H7B	110.4	C31—C36—C35	120.6 (4)
P1—C7—H7B	110.4	C31—C36—H36	119.7
H7A—C7—H7B	108.6	C35—C36—H36	119.7
C6—C8—P2	106.5 (2)	C46—C41—C42	117.8 (3)
C6—C8—H8A	110.4	C46—C41—P2	119.4 (3)
P2—C8—H8A	110.4	C42—C41—P2	122.8 (3)
C6—C8—H8B	110.4	C41—C42—C43	118.9 (4)
P2—C8—H8B	110.4	C41—C42—H42	120.6
H8A—C8—H8B	108.6	C43—C42—H42	120.6
C16—C11—C12	117.5 (3)	C44—C43—C42	121.7 (4)
C16—C11—P1	119.2 (3)	C44—C43—H43	119.1
C12—C11—P1	123.2 (3)	C42—C43—H43	119.1
C13—C12—C11	120.8 (4)	C43—C44—C45	119.0 (4)
C13—C12—H12	119.6	C43—C44—H44	120.5
C11—C12—H12	119.6	C45—C44—H44	120.5
C14—C13—C12	120.5 (4)	C44—C45—C46	120.3 (4)
C14—C13—H13	119.7	C44—C45—H45	119.9
C12—C13—H13	119.7	C46—C45—H45	119.9
C13—C14—C15	119.8 (4)	C45—C46—C41	122.3 (4)
C13—C14—H14	120.1	C45—C46—H46	118.9
C15—C14—H14	120.1	C41—C46—H46	118.9