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Crystals of the title compound, [PtCl2(C27H36N3P)2], as the trans-isomer were obtained from the originally formed cis-isomer after standing for more than four months in solution. In the crystal structure, the Pt atom is located on an inversion centre, which makes the mol­ecular structure similar to the triphenyl­phosphine analogue. The amino groups are pyramidal and do not inter­act with Pt atoms or hydrogen-bond donors.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805038882/bt6791sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805038882/bt6791Isup2.hkl
Contains datablock I

CCDC reference: 293842

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.020
  • wR factor = 0.050
  • Data-to-parameter ratio = 20.4

checkCIF/PLATON results

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Alert level C CRYSC01_ALERT_1_C The word below has not been recognised as a standard identifier. yellowish CRYSC01_ALERT_1_C No recognised colour has been given for crystal colour. PLAT141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT142_ALERT_4_C su on b - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT143_ALERT_4_C su on c - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT145_ALERT_4_C su on beta Small or Missing (x 10000) ..... 4 Deg. PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.86 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.04 Ratio
0 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 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 4 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1999); cell refinement: HKL-2000 (Otwinowski & Minor, 1997); data reduction: HKL-2000, DENZOX (Farrugia, 2004) and SADABS (Sheldrick, 2002); 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: manually editing SHELXL97 output.

trans-Dichlorobis(tris{4-[(dimethylamino)methyl]phenyl}phosphine)platinum(II) top
Crystal data top
[PtCl2(C27H36N3P)2]F(000) = 1160
Mr = 1133.11Dx = 1.407 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 43969 reflections
a = 13.1122 (1) Åθ = 1.0–27.5°
b = 17.6200 (1) ŵ = 2.82 mm1
c = 11.6180 (1) ÅT = 150 K
β = 94.9554 (4)°Block, yellowish
V = 2674.16 (3) Å30.27 × 0.09 × 0.09 mm
Z = 2
Data collection top
Nonius KappaCCD
diffractometer
6131 independent reflections
Radiation source: rotating anode5028 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
φ and ω scansθmax = 27.5°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
h = 1717
Tmin = 0.62, Tmax = 0.78k = 2222
57383 measured reflectionsl = 1515
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)] = 0.020Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.050H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0197P)2 + 2.3473P]
where P = (Fo2 + 2Fc2)/3
6131 reflections(Δ/σ)max = 0.001
301 parametersΔρmax = 0.84 e Å3
0 restraintsΔρmin = 0.50 e Å3
Special details top

Experimental. The X-ray intensities were obtained with two different exposure times and rotation angles of 1°. 363 φ and 334 ω scans were measured with an exposure time of 40 s per frame; 206 φ and 90 ω scans with an exposure time of 8 s per frame. The frames were integrated with DENZO (Otwinowski & Minor, 1997) and the resulting files were converted with DENZOX (Farrugia, 2004). The resulting file was scaled and corrected for absorption with SADABS (Sheldrick, 2002).

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
Pt10.50000.50000.50000.01778 (4)
Cl10.67425 (4)0.51413 (3)0.53872 (5)0.02918 (13)
P10.50904 (4)0.51907 (3)0.30349 (5)0.01878 (11)
N10.20169 (17)0.23248 (12)0.0739 (2)0.0389 (5)
N20.21225 (15)0.77656 (11)0.01699 (18)0.0321 (5)
N31.02199 (15)0.52548 (13)0.23664 (18)0.0321 (5)
C110.43711 (16)0.44688 (12)0.21934 (18)0.0205 (4)
C120.37972 (17)0.46236 (13)0.11618 (19)0.0236 (5)
H120.37350.51310.08890.028*
C130.33130 (17)0.40397 (13)0.05250 (19)0.0264 (5)
H130.29170.41560.01770.032*
C140.33928 (17)0.32905 (13)0.0888 (2)0.0270 (5)
C150.39626 (19)0.31364 (13)0.1932 (2)0.0317 (5)
H150.40280.26280.22020.038*
C160.44340 (18)0.37193 (13)0.2578 (2)0.0291 (5)
H160.48070.36060.32950.035*
C170.2852 (2)0.26743 (14)0.0170 (2)0.0362 (6)
H17A0.25730.28920.05770.043*
H17B0.33540.22780.00060.043*
C180.1293 (2)0.28785 (18)0.1088 (3)0.0569 (9)
H18A0.10190.31690.04110.085*
H18B0.16380.32240.16570.085*
H18C0.07320.26190.14300.085*
C190.1498 (2)0.17720 (16)0.0053 (3)0.0503 (8)
H19A0.09450.15270.03250.075*
H19B0.19910.13870.02590.075*
H19C0.12130.20320.07530.075*
C210.45621 (16)0.61024 (12)0.25173 (18)0.0199 (4)
C220.46979 (17)0.63671 (12)0.14063 (19)0.0233 (5)
H220.51550.61120.09470.028*
C230.41679 (17)0.70013 (12)0.09704 (19)0.0245 (5)
H230.42650.71760.02140.029*
C240.34945 (17)0.73839 (12)0.16345 (19)0.0238 (5)
C250.34154 (18)0.71457 (12)0.27606 (19)0.0263 (5)
H250.30000.74240.32420.032*
C260.39363 (17)0.65051 (13)0.31955 (19)0.0252 (5)
H260.38610.63440.39640.030*
C270.28317 (18)0.80230 (12)0.1129 (2)0.0273 (5)
H27A0.24380.82410.17390.033*
H27B0.32740.84280.08540.033*
C280.1540 (2)0.84024 (16)0.0341 (2)0.0413 (6)
H28A0.11010.82270.10140.062*
H28B0.20110.87910.05840.062*
H28C0.11140.86190.02300.062*
C290.1430 (2)0.71944 (16)0.0549 (3)0.0542 (8)
H29A0.10380.74070.11540.081*
H29B0.18250.67560.08580.081*
H29C0.09600.70330.01060.081*
C310.63528 (16)0.51560 (12)0.24951 (18)0.0210 (4)
C320.70435 (17)0.57466 (13)0.27647 (19)0.0240 (5)
H320.68350.61760.31790.029*
C330.80304 (17)0.57073 (13)0.24299 (19)0.0262 (5)
H330.84910.61150.26100.031*
C340.83605 (17)0.50777 (13)0.18317 (19)0.0258 (5)
C350.76676 (18)0.45011 (13)0.1554 (2)0.0276 (5)
H350.78760.40730.11370.033*
C360.66731 (17)0.45368 (13)0.18719 (19)0.0251 (5)
H360.62070.41370.16640.030*
C370.94398 (18)0.50366 (14)0.1470 (2)0.0303 (5)
H37A0.95760.45110.12260.036*
H37B0.94910.53710.07930.036*
C381.1225 (2)0.52303 (17)0.1910 (3)0.0423 (7)
H38A1.17490.54010.25060.063*
H38B1.12240.55640.12350.063*
H38C1.13750.47090.16830.063*
C391.0225 (2)0.47619 (19)0.3361 (2)0.0462 (7)
H39A1.03420.42370.31250.069*
H39B0.95640.47970.36920.069*
H39C1.07730.49180.39400.069*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.01637 (6)0.02192 (6)0.01461 (6)0.00011 (5)0.00116 (4)0.00174 (4)
Cl10.0166 (2)0.0482 (4)0.0221 (3)0.0029 (2)0.0021 (2)0.0053 (2)
P10.0175 (3)0.0239 (3)0.0146 (3)0.0008 (2)0.0008 (2)0.0012 (2)
N10.0358 (12)0.0298 (11)0.0488 (14)0.0043 (9)0.0097 (10)0.0056 (10)
N20.0300 (11)0.0310 (11)0.0342 (12)0.0075 (9)0.0027 (9)0.0008 (9)
N30.0224 (10)0.0424 (11)0.0319 (11)0.0022 (9)0.0042 (9)0.0026 (9)
C110.0174 (10)0.0244 (10)0.0194 (11)0.0003 (8)0.0003 (8)0.0013 (8)
C120.0248 (11)0.0250 (12)0.0209 (11)0.0017 (9)0.0009 (9)0.0021 (9)
C130.0263 (12)0.0333 (12)0.0185 (11)0.0012 (10)0.0039 (9)0.0002 (9)
C140.0241 (12)0.0303 (12)0.0264 (12)0.0006 (10)0.0016 (9)0.0052 (9)
C150.0371 (14)0.0224 (11)0.0342 (14)0.0008 (10)0.0045 (11)0.0009 (10)
C160.0306 (13)0.0303 (12)0.0244 (12)0.0025 (10)0.0097 (10)0.0022 (9)
C170.0437 (15)0.0308 (13)0.0327 (14)0.0046 (11)0.0052 (12)0.0069 (11)
C180.0369 (16)0.0494 (18)0.084 (3)0.0069 (14)0.0022 (16)0.0145 (17)
C190.0481 (17)0.0354 (15)0.063 (2)0.0073 (13)0.0222 (15)0.0065 (14)
C210.0195 (10)0.0213 (10)0.0181 (11)0.0014 (8)0.0035 (8)0.0018 (8)
C220.0227 (11)0.0274 (11)0.0206 (11)0.0005 (9)0.0056 (9)0.0008 (9)
C230.0278 (12)0.0266 (11)0.0193 (11)0.0016 (9)0.0026 (9)0.0049 (9)
C240.0258 (11)0.0219 (11)0.0234 (11)0.0012 (9)0.0002 (9)0.0006 (9)
C250.0307 (12)0.0260 (11)0.0227 (12)0.0044 (10)0.0056 (9)0.0027 (9)
C260.0296 (12)0.0283 (12)0.0180 (11)0.0020 (9)0.0033 (9)0.0003 (9)
C270.0297 (12)0.0232 (11)0.0292 (13)0.0011 (9)0.0029 (10)0.0022 (9)
C280.0312 (14)0.0454 (16)0.0466 (17)0.0104 (12)0.0005 (12)0.0085 (13)
C290.0404 (17)0.0379 (16)0.081 (2)0.0069 (13)0.0147 (16)0.0055 (15)
C310.0185 (10)0.0299 (12)0.0143 (10)0.0014 (8)0.0001 (8)0.0043 (8)
C320.0251 (11)0.0270 (11)0.0196 (11)0.0010 (9)0.0003 (9)0.0019 (9)
C330.0234 (11)0.0338 (12)0.0210 (11)0.0056 (9)0.0003 (9)0.0005 (9)
C340.0212 (11)0.0391 (13)0.0171 (10)0.0067 (10)0.0018 (8)0.0073 (9)
C350.0293 (12)0.0301 (12)0.0236 (12)0.0055 (10)0.0043 (10)0.0012 (9)
C360.0269 (12)0.0264 (11)0.0218 (11)0.0011 (9)0.0016 (9)0.0009 (9)
C370.0239 (11)0.0442 (14)0.0234 (11)0.0043 (10)0.0050 (9)0.0022 (10)
C380.0265 (13)0.0533 (16)0.0474 (17)0.0036 (12)0.0048 (12)0.0030 (13)
C390.0354 (15)0.0656 (19)0.0366 (16)0.0034 (14)0.0021 (12)0.0151 (14)
Geometric parameters (Å, º) top
Pt1—Cl12.3038 (5)C22—C231.388 (3)
Pt1—Cl1i2.3038 (5)C22—H220.9500
Pt1—P1i2.3207 (5)C23—C241.396 (3)
Pt1—P12.3208 (5)C23—H230.9500
P1—C111.818 (2)C24—C251.386 (3)
P1—C211.830 (2)C24—C271.510 (3)
P1—C311.821 (2)C25—C261.391 (3)
N1—C181.443 (4)C25—H250.9500
N1—C171.463 (3)C26—H260.9500
N1—C191.466 (3)C27—H27A0.9900
N2—C291.449 (4)C27—H27B0.9900
N2—C281.455 (3)C28—H28A0.9800
N2—C271.461 (3)C28—H28B0.9800
N3—C391.445 (3)C28—H28C0.9800
N3—C371.447 (3)C29—H29A0.9800
N3—C381.463 (3)C29—H29B0.9800
C11—C121.386 (3)C29—H29C0.9800
C11—C161.394 (3)C31—C361.394 (3)
C12—C131.388 (3)C31—C321.397 (3)
C12—H120.9500C32—C331.385 (3)
C13—C141.387 (3)C32—H320.9500
C13—H130.9500C33—C341.398 (3)
C14—C151.395 (3)C33—H330.9500
C14—C171.509 (3)C34—C351.382 (3)
C15—C161.385 (3)C34—C371.512 (3)
C15—H150.9500C35—C361.387 (3)
C16—H160.9500C35—H350.9500
C17—H17A0.9900C36—H360.9500
C17—H17B0.9900C37—H37A0.9900
C18—H18A0.9800C37—H37B0.9900
C18—H18B0.9800C38—H38A0.9800
C18—H18C0.9800C38—H38B0.9800
C19—H19A0.9800C38—H38C0.9800
C19—H19B0.9800C39—H39A0.9800
C19—H19C0.9800C39—H39B0.9800
C21—C261.382 (3)C39—H39C0.9800
C21—C221.398 (3)
Cl1—Pt1—Cl1i180.0C24—C23—H23119.7
Cl1—Pt1—P1i87.573 (19)C25—C24—C23118.5 (2)
Cl1i—Pt1—P1i92.429 (19)C25—C24—C27120.4 (2)
Cl1—Pt1—P192.430 (19)C23—C24—C27121.0 (2)
Cl1i—Pt1—P187.569 (19)C24—C25—C26120.9 (2)
P1i—Pt1—P1180.0C24—C25—H25119.5
C11—P1—C31103.66 (10)C26—C25—H25119.5
C11—P1—C21105.87 (9)C21—C26—C25120.4 (2)
C31—P1—C21104.23 (10)C21—C26—H26119.8
C11—P1—Pt1111.07 (7)C25—C26—H26119.8
C31—P1—Pt1117.33 (7)N2—C27—C24111.86 (18)
C21—P1—Pt1113.60 (7)N2—C27—H27A109.2
C18—N1—C17112.2 (2)C24—C27—H27A109.2
C18—N1—C19110.2 (2)N2—C27—H27B109.2
C17—N1—C19108.7 (2)C24—C27—H27B109.2
C29—N2—C28109.8 (2)H27A—C27—H27B107.9
C29—N2—C27111.0 (2)N2—C28—H28A109.5
C28—N2—C27110.5 (2)N2—C28—H28B109.5
C39—N3—C37111.7 (2)H28A—C28—H28B109.5
C39—N3—C38109.2 (2)N2—C28—H28C109.5
C37—N3—C38109.5 (2)H28A—C28—H28C109.5
C12—C11—C16118.4 (2)H28B—C28—H28C109.5
C12—C11—P1123.03 (16)N2—C29—H29A109.5
C16—C11—P1118.48 (16)N2—C29—H29B109.5
C11—C12—C13120.3 (2)H29A—C29—H29B109.5
C11—C12—H12119.9N2—C29—H29C109.5
C13—C12—H12119.9H29A—C29—H29C109.5
C14—C13—C12121.6 (2)H29B—C29—H29C109.5
C14—C13—H13119.2C36—C31—C32118.7 (2)
C12—C13—H13119.2C36—C31—P1121.92 (17)
C13—C14—C15118.1 (2)C32—C31—P1119.25 (16)
C13—C14—C17119.8 (2)C33—C32—C31120.2 (2)
C15—C14—C17122.1 (2)C33—C32—H32119.9
C16—C15—C14120.5 (2)C31—C32—H32119.9
C16—C15—H15119.8C32—C33—C34121.1 (2)
C14—C15—H15119.8C32—C33—H33119.5
C15—C16—C11121.2 (2)C34—C33—H33119.5
C15—C16—H16119.4C35—C34—C33118.3 (2)
C11—C16—H16119.4C35—C34—C37120.8 (2)
N1—C17—C14112.8 (2)C33—C34—C37120.9 (2)
N1—C17—H17A109.0C34—C35—C36121.2 (2)
C14—C17—H17A109.0C34—C35—H35119.4
N1—C17—H17B109.0C36—C35—H35119.4
C14—C17—H17B109.0C35—C36—C31120.4 (2)
H17A—C17—H17B107.8C35—C36—H36119.8
N1—C18—H18A109.5C31—C36—H36119.8
N1—C18—H18B109.5N3—C37—C34114.08 (19)
H18A—C18—H18B109.5N3—C37—H37A108.7
N1—C18—H18C109.5C34—C37—H37A108.7
H18A—C18—H18C109.5N3—C37—H37B108.7
H18B—C18—H18C109.5C34—C37—H37B108.7
N1—C19—H19A109.5H37A—C37—H37B107.6
N1—C19—H19B109.5N3—C38—H38A109.5
H19A—C19—H19B109.5N3—C38—H38B109.5
N1—C19—H19C109.5H38A—C38—H38B109.5
H19A—C19—H19C109.5N3—C38—H38C109.5
H19B—C19—H19C109.5H38A—C38—H38C109.5
C26—C21—C22118.96 (19)H38B—C38—H38C109.5
C26—C21—P1119.33 (16)N3—C39—H39A109.5
C22—C21—P1121.43 (16)N3—C39—H39B109.5
C23—C22—C21120.4 (2)H39A—C39—H39B109.5
C23—C22—H22119.8N3—C39—H39C109.5
C21—C22—H22119.8H39A—C39—H39C109.5
C22—C23—C24120.5 (2)H39B—C39—H39C109.5
C22—C23—H23119.7
Pt1—P1—C11—C1641.2 (2)C31—P1—C21—C26145.38 (18)
Pt1—P1—C21—C2616.5 (2)C11—P1—C21—C2268.3 (2)
Pt1—P1—C31—C3271.20 (18)C31—P1—C21—C2240.7 (2)
C19—N1—C17—C14176.3 (2)Pt1—P1—C21—C22169.60 (15)
C28—N2—C27—C24176.6 (2)C26—C21—C22—C233.5 (3)
C38—N3—C37—C34177.3 (2)P1—C21—C22—C23170.45 (17)
C15—C14—C17—N166.2 (3)C21—C22—C23—C240.1 (3)
C23—C24—C27—N262.1 (3)C22—C23—C24—C253.9 (3)
C33—C34—C37—N345.6 (3)C22—C23—C24—C27173.6 (2)
Cl1—Pt1—P1—C11132.12 (8)C23—C24—C25—C264.7 (3)
Cl1i—Pt1—P1—C1147.89 (8)C27—C24—C25—C26172.8 (2)
Cl1—Pt1—P1—C3113.17 (8)C22—C21—C26—C252.7 (3)
Cl1i—Pt1—P1—C31166.83 (8)P1—C21—C26—C25171.32 (17)
Cl1—Pt1—P1—C21108.67 (8)C24—C25—C26—C211.4 (3)
Cl1i—Pt1—P1—C2171.32 (8)C29—N2—C27—C2461.4 (3)
C31—P1—C11—C1291.54 (19)C25—C24—C27—N2115.4 (2)
C21—P1—C11—C1217.9 (2)C11—P1—C31—C3617.6 (2)
Pt1—P1—C11—C12141.60 (17)C21—P1—C31—C36128.19 (18)
C31—P1—C11—C1685.7 (2)Pt1—P1—C31—C36105.23 (17)
C21—P1—C11—C16164.94 (18)C11—P1—C31—C32165.98 (17)
C16—C11—C12—C131.0 (3)C21—P1—C31—C3255.37 (19)
P1—C11—C12—C13176.22 (17)C36—C31—C32—C330.9 (3)
C11—C12—C13—C140.6 (4)P1—C31—C32—C33175.63 (17)
C12—C13—C14—C151.2 (4)C31—C32—C33—C340.8 (3)
C12—C13—C14—C17179.9 (2)C32—C33—C34—C351.7 (3)
C13—C14—C15—C160.2 (4)C32—C33—C34—C37179.8 (2)
C17—C14—C15—C16178.9 (2)C33—C34—C35—C361.0 (3)
C14—C15—C16—C111.4 (4)C37—C34—C35—C36179.4 (2)
C12—C11—C16—C152.0 (4)C34—C35—C36—C310.7 (3)
P1—C11—C16—C15175.38 (19)C32—C31—C36—C351.7 (3)
C18—N1—C17—C1454.2 (3)P1—C31—C36—C35174.80 (17)
C13—C14—C17—N1112.5 (3)C39—N3—C37—C3461.6 (3)
C11—P1—C21—C26105.64 (18)C35—C34—C37—N3136.0 (2)
Symmetry code: (i) x+1, y+1, z+1.
 

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